• Title/Summary/Keyword: tertiary amine

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Study on the extraction mechanism and the optimization of extraction method for Chromium using anion exchangers (음이온 교환체를 이용한 크롬의 추출메카니즘 및 추출방법 최적화에 관한 연구)

  • Kim, S.W.;Kim, D.M.;Kim, Y.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.387-393
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    • 1994
  • Quantitative analytical conditions for chromium using solvent extraction followed by atomic absorption spectrometry was studied. Trioctylamine(TOA) in tertiary amine or Trioctylmethylammoniumchloride(TOMAC) in quaternary ammonium salt, both containing octyl group was used as an anion exchangers. Absorbance were measured for the different kinds of acid added and as changing the concentration of acid by graphite furnace atomic absorption spectrometer. The maximum absorbance was obtained at the concentrations of HCl, 0.1M to 0.3M for TOA and 0.03M to 0.1M for TOMAC. Mole ratios over 1:1 of TOA or TOMAC dissolved in MIBK solution to chromium in sample shows optimum extraction efficiency while HCl was added to the MIBK. As a result of scrutinizing the extraction process, the methods employed in this experiment turned out to be better extraction efficiency for chromium, compared to similar extraction methods.

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Reaction of Lithium Tris(diethylamino)aluminum Hydride in Tetrahydrofuran with Selected Organic Compounds Containing Representative Functional Groups

  • Jin Soon Cha;Jae Cheol Lee
    • Bulletin of the Korean Chemical Society
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    • v.14 no.4
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    • pp.469-475
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    • 1993
  • The approximate rates and stoichiometry of the reaction of excess lithium tris(diethylamino)aluminum hydride (LTDEA) with selected organic compounds containing representative functional groups under standardized condition (tetrahydrofuran, 0$^{\circ}C$) were examined in order to define the characteristics of the reagent for selective reductions. The reducing ability of LTDEA was also compared with those of the parent lithium aluminum hydride (LAH) and lithium tris(dibutylamino)aluminum hydride (LTDBA). In general, the reactivity toward organic functionalities is in order of LAH${\gg}$LTDEA${\geq}$LTDBA. LTDEA shows a unique reducing characteristics. Thus, benzyl alcohol and phenol evolve hydrogen slowly. The rate of hydrogen evolution of primary, secondary, and tertiary alcohols is distinctive: 1-hexanol evolves hydrogen completely in 6 h, whereas 3-hexanol evolves hydrogen very slowly. However, 3-ethyl-3-pentanol does not evolve any hydrogen under these reaction conditions. Primary amine, such as n-hexylamine, evolves only 1 equivalent of hydrogen. On the other hand, thiols examined are absolutely inert to this reagent. LTDEA reduces aldehydes, ketones, esters, acid chlorides, and epoxides readily to the corresponding alcohols. Quinones, such as p-benzoquinone and anthraquinone, are reduced to the corresponding diols without hydrogen evolution. However, carboxylic acids, anhydrides, nitriles, and primary amides are reduced slowly, where as tertiary amides are readily reduced. Finally, sulfides and sulfoxides are reduced to thiols and sulfides, respectively, without evolution of hydrogen. In addition to that, the reagent appears to be an excellent partial reducing agent to convert esters, primary carboxamides, and aromatic nitriles into the corresponding aldehydes. Free carboxylic acids are also converted into aldehydes through treatment of acyloxy-9-BBN with this reagent in excellent yields.

Reducing Characteristics of Potassium Triethylborohydride

  • Yoon, Nung-Min;Yang H.S.;Hwang, Y.S.
    • Bulletin of the Korean Chemical Society
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    • v.8 no.4
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    • pp.285-291
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    • 1987
  • The approximate rates, stoichiometries and products of the reaction of potassium triethylborohydride $(KEt_3BH)$ with selected organic compounds containing representative functional groups under the standard condition $(0^{\circ}C,$ THF) were examined in order to explore the reducing characteristics of this reagent as a selective reducing agent. Primary alcohols, phenols and thiols evolve hydrogen rapidly whereas secondary and tertiary alcohols evolve very slowly. n-Hexylamine is inert to this reagent. Aldehydes and ketones are reduced rapidly and quantitatively to the corresponding alcohols. Reduction of noncamphor gives 3% exo- and 97% endo-norboneol. Anthraquinone is cleanly reduced to 9,10-dihydro-9,10-dihydroxyanthracene stage. Carboxylic acids liberate hydrogen rapidly and quantitatively but further reduction does not occur. Anhydrides utilize 2 equiv of hydride to give an equimolar mixture of acid and alcohol. Acid chlorides, esters and lactones are rapidly and quantitatively reduced to the corresponding alcohols. Epoxides are reduced at moderate rates with Markovnikov ring opening to give the more substituted alcohols. Primary amides liberate 1 equiv of hydrogen rapidly. Further reduction of caproamide is slow whereas benzamide is not reduced. Tertiary amides are reduced slowly. Benzonitrile utilizes 2 equiv of hydride in 3 h to go to the amine stage whereas capronitrile takes only 1 equiv. The reaction of nitro compounds undergo rapidly whereas azobenzene and azoxybenzene are reduced slowly. Cyclohexanone oxime rapidly evolves hydrogen without reduction. Phenyl isocyanate utilizes 1 equiv of hydride to proceed to formanilide stage. Pyridine N-oxide and pyridine is reduced rapidly. Disulfides are rapidly reduced to the thiol stage whereas sulfoxide, sulfonic acid are practically inert to this reagent. Sulfones and cyclohexyl tosylate are slowly reduced. Octyl bromide is reduced rapidly but octyl chloride and cyclohexyl bromide are reduced slowly.

A study on the Property of Oxidation Stability in Biodiesel by the Additives (첨가제에 따른 바이오디젤 산화안정 특성 연구)

  • Kang, Hyung-Kyu;Song, Ho-Yong;Doe, Jin-Woo;Park, Soo-Youl;Na, Byung-Ki
    • Journal of the Korean Applied Science and Technology
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    • v.32 no.4
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    • pp.639-648
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    • 2015
  • Some materials of fatty acids in the biodiesel affect the physical/chemical properties like density, kinematic viscosity, total acid number and oxidation stability by forming an organic fatty acid in combination with oxygen in the air. To solve the problem of the oxidative stability of biodiesel, various kinds of antioxidant has added and analyze the characteristics of the physical/chemical property changes by the addition of antioxidant. Oxidation stability increased by the increase of additives content. The TBHQ among the seven kinds of the additives showed the best performance. Also, 4 kinds of additives like propyl gallate, butyl-amine and pyrogallo has showed above 10 hr of oxidation stability at the addition of 500 ppm. In case of pyrogallo, this is not appropriate as an additive to suitable quality standards of total acid number. TBHA, DTBHQ of hydroquinone was satisfied with the quality standard of oxidation stability but the target of this research(above 10 hr) did not satisfied with oxidation stability. Propyl gallate is also a suitable at the quality standards of total acid number but it was shown not to be an appropriate to the additives due to increasing the total acid number by increasing of the content of additives at the addition of 500 ppm.

Precise Control of Thermoresponsive Properties of Polymers with Hydroxy Groups in the Side Chains (곁가지에 다양한 길이의 알코올 그룹을 지닌 고분자들의 저임계 용액온도 민감성 제어)

  • Lee, Hyung-Il
    • Polymer(Korea)
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    • v.39 no.1
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    • pp.165-168
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    • 2015
  • Thermoresponsive polymers were successfully synthesized by a combination of atom transfer radical polymerization (ATRP) and Cu(I)-catalyzed 1,3-dipolar cycloaddition of azide and alkynes (click chemistry). Poly(2-hydroxyethyl methacrylate) (PHEMA) was synthesized by ATRP, followed by introduction of alkyne groups using pentynoic acid, leading to HEMA-alkyne. Homopolymers having secondary amine groups, tertiary amines with hydroxyethyl and hydroxypropyl groups were synthesized by adding 2-azido-N-ethyl-ethanamine, 2-[(2-azidoethyl)amino]ethanol, and 2-[(2-azidoethyl)amino]propanol, respectively, to the PHEMA-alkyne backbone using click chemistry. Molecular weight (MW), molecular weight distribution (MWD), and click reaction efficiency were determined by gel permeation chromatography (GPC) and $^1H$ NMR spectroscopy. The transmission spectra of the 1.0 wt% aqueous solutions of the resulting polymers at 650 nm were measured as a function of temperature. Results showed that the lower critical solution temperature (LCST) could be easily controlled by the length of the hydroxyalkyl groups.

Preparation and Properties of Novel Biodegradable Hydrogel based on Cationic Polyaspartamide Derivative

  • Moon, Jong-Rok;Kim, Bong-Seop;Kim, Ji-Heung
    • Bulletin of the Korean Chemical Society
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    • v.27 no.7
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    • pp.981-985
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    • 2006
  • Novel copolymers consisting of poly(2-hydroxyethyl aspartamide-co-N,N'-dimethyl-1,3-propane aspartamide) (PHEA-DPA) were prepared from polysuccinimide (PSI), which is the thermal polycondensation product of aspartic acid, via a ring-opening reaction with N,N'-dimethyl-1,3-propane diamine (DPA) and ethanolamine. The prepared water-soluble copolymer was then crosslinked by reacting it with hexamethylene diisocyanate to provide the corresponding gel. The swelling behavior and morphology of the crosslinked hydrogels were investigated. The degree of swelling decreased with increasing crosslinking reagent due to the higher crosslinking density. It was also confirmed that the swelling property is affected by pH. At low pH (< pH 4), swelling is increased due to the ionization of DPA with a tertiary amine moiety. In addition, a reversible swelling and de-swelling behavior was demonstrated by adjusting the pH of the solution. The prepared hydrogels showed a well-interconnected microporous structure with regular 5-20 $\mu$m sized pores.

Synthesis and Characterization of Mononuclear Octahedral Fe(III) Complex Containing a Biomimetic Tripodal Ligand, N-(Benzimidazol-2-ylmethyl)iminodiacetic Acid

  • Moon, Do-Hyun;Kim, Jung-hyun;Lah, Myoung-Soo
    • Bulletin of the Korean Chemical Society
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    • v.27 no.10
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    • pp.1597-1600
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    • 2006
  • The mononuclear iron complex 1, $Fe^{III}$(Hbida)Cl($H_2O$), was synthesized using a tripodal tetradentate ligand, N-(benzimidazol-2-ylmethyl)iminodiacetic acid (H3bida), which has two carboxylate groups, one benzimida- zoyl group, and one tertiary amine where it serves as a tetradentate chelating ligand for the octahedral Fe(III) ion. The four equatorial positions of the octahedral complex are occupied by two monodentate carboxylates, a benzimidazole nitrogen, and an oxygen of a water molecule. One of the axial positions is occupied by an apical nitrogen of the Hbida and the other by a chloride anion. The mononuclear octahedral complex 1 mimics the geometry of the key intermediate structure of the catalytic reaction cycle proposed for the FeSODs, which is a distorted octahedral geometry with three histidyl imidazoles, an aspartyl carboxylate, a superoxide anion, and a water molecule. The redox potential of complex 1, $E_{1/2}$ is -0.11V vs. Ag/AgCl (0.12 V vs. NHE), which is slightly lower than those reported for the most FeSODs. The magnetic susceptibility of complex 1 at room temperature is 5.83 $\mu$B which is close to that of the spin only value, 5.92 $\mu$B of high-spin d5 Fe(III).

Effect of Photo-accelerator on the Dental Properties of Acryl-based Polymeric Dental Restorative Composites (아크릴계 고분자 치아수복재의 치과적 물성에 미치는 광증감제 효과)

  • Kim, Ohyoung
    • Applied Chemistry for Engineering
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    • v.16 no.1
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    • pp.117-122
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    • 2005
  • The aim of this study was to evaluate the effect of tertiary amine photo-accelerator on the dental properties of visible light-activated, polymeric, dental restorative composites (PDRC) through the measurement of mechanical and esthetic properties. The surface of barium silicate was hydrophobically treated to improve the interfacial behavior with the acrylic resin matrix. Camphorquinone was adopted as a photo-initiator with 0.5 wt% based on the resin matrix. It was discovered that the dental properties of PDRC were primarily dependent on the chemical structure rather than the added content of photo-accelerator.

Recovery of Molybdenum from the Desulfurizing Spent Catalyst (석유 탈황 폐촉매로부터 몰리브덴의 회수에 관한 연구)

  • 김종화;서명교;양종규;김준수
    • Resources Recycling
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    • v.7 no.2
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    • pp.9-15
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    • 1998
  • Recovery af molybdenum in spent desulfuriring catalyst of petrochemical industries was studied from MfGnatc solulion which is a resultant of firstly remvercd vanadium by wet processes. In order to separate and recover molybdenum from upper mentioned rafinatz solution containing several mctal ions, such as molybdenum (1,100 ppm), vanadium (150 ppm), aluminium (19 ppm), and nickel (33 ppm), either adsorption technique by chelate resin or solvent extr~ction by tertiary amine as extractant was applied. In case of adsorption method, palyamine type chelate resin showed the highest selectivily far molybdenum ion up lo 60 ddm' of ancentration aftcr eluting with 3.0 rnolld~n' of NH,OH. On the othcr hand. molybdenum ion wa cffectlvely cxtractcd in Ule whole ranges of equilibrilrm pR by solvent extraction method with 10 ~01%-alamine 336 which was pretreated with 2N-HCI

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Preparation of Quaternary Ammonium Salt Derivatives Supported on Silica gel and Its Ion Exchange Characteristics (실리카겔에 담지된 4급암모늄염 유도체의 합성 및 이온교환 특성)

  • Ahn, Beom-Shu
    • Journal of the Korean Applied Science and Technology
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    • v.25 no.1
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    • pp.65-72
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    • 2008
  • The ion exchangers supported on silica gel containing primary, secondary, or tertiary amine groups show a behaviour that is weakly acidic, while the quaternary salts are strongly acidic. These properties change according to the hydrophilicities of the modifier functional groups. Ammonium salt derivatives supported on silica gel were prepared from silica modified with 3-Aminopropyltriethoxysiliane and N-3-(Trimethoxysilyl)propylehtylene diamine. The preparation and the ion exchange properties of two systems were discussed. Two systems have different hydrophilicities and contain ammonium chloride derivatives of 3-amminopropyltriethoxysilane and N-3-(triehtoxysilyl)propyl ethylene diamine supported on silica gel, $SA^+/Cl^-$ and $SA^+/Cl^-$, respectively. The high affinity to perchlorate ion presented by the $SA^+/Cl^-$ through the equilibrium studies of ion exchange led us to its application as an ion selective electrode for the perchlorate ion. The determination of the perchlorate ion in the presence of other anions and in complexes is very difficult. Few analytical methods are available and most of them are indirect. Both materials showed potential use as an ion exchanger; they are thermically stable, achieve equilibrium rapidly in the presence of suitable exchanger ions, and are easily recovered.