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Phases containing intermediate

Hydrochloric acid [7647-01-0], which is formed as by-product from unreacted chloroacetic acid, is fed into an absorption column. After the addition of acid and alcohol is complete, the mixture is heated at reflux for 6—8 h, whereby the intermediate malonic acid ester monoamide is hydroly2ed to a dialkyl malonate. The pure ester is obtained from the mixture of cmde esters by extraction with ben2ene [71-43-2], toluene [108-88-3], or xylene [1330-20-7]. The organic phase is washed with dilute sodium hydroxide [1310-73-2] to remove small amounts of the monoester. The diester is then separated from solvent by distillation at atmospheric pressure, and the malonic ester obtained by redistillation under vacuum as a colorless Hquid with a minimum assay of 99%. The aqueous phase contains considerable amounts of mineral acid and salts and must be treated before being fed to the waste treatment plant. The process is suitable for both the dimethyl and diethyl esters. The yield based on sodium chloroacetate is 75—85%. Various low molecular mass hydrocarbons, some of them partially chlorinated, are formed as by-products. Although a relatively simple plant is sufficient for the reaction itself, a si2eable investment is required for treatment of the wastewater and exhaust gas. [Pg.467]

Thus, RP-HPLC-MS has been employed for the analysis of sulphonated dyes and intermediates. Dyes included in the investigation were Acid yellow 36, Acid blue 40, Acid violet 7, Direct yellow 28, Direct blue 106, Acid yellow 23, Direct green 28, Direct red 79, Direct blue 78 and some metal complex dyes such as Acid orange 142, Acid red 357, Acid Violet 90, Acid yellow 194 and Acid brown 355. RP-HPLC was realized in an ODS column (150 X 3 mm i.d. particle size 7 /.an). The composition of the mobile phase varied according to the chemical structure of the analytes to be separated. For the majority of cases the mobile phase consisted of methanol-5 mM aqueous ammonium acetate (10 90, v/v). Subsituted anthraquinones were separated in similar mobile phases containing 40 per cent methanol. The flow rate was 1 ml/min for UV and 0.6 ml/min for MS detection, respectively. The chemical structure of dye intermediates investigated in this study and their retention times are compiled in Table 3.28. It was found that the method is suitable for the separation of decomposition products and intermediates of dyes but the separation of the original dye molecules was not adequate in this RP-HPLC system [162],... [Pg.484]

Peterson and Scarrah 165) reported the transesterification of rapeseed oil by methanol in the presence of alkaline earth metal oxides and alkali metal carbonates at 333-336 K. They found that although MgO was not active for the transesterification reaction, CaO showed activity, which was enhanced by the addition of MgO. In contrast, Leclercq et al. 166) showed that the methanolysis of rapeseed oil could be carried out with MgO, although its activity depends strongly on the pretreatment temperature of this oxide. Thus, with MgO pre-treated at 823 K and a methanol to oil molar ratio of 75 at methanol reflux, a conversion of 37% with 97% selectivity to methyl esters was achieved after 1 h in a batch reactor. The authors 166) showed that the order of activity was Ba(OH)2 > MgO > NaCsX zeolite >MgAl mixed oxide. With the most active catalyst (Ba(OH)2), 81% oil conversion, with 97% selectivity to methyl esters after 1 h in a batch reactor was achieved. Gryglewicz 167) also showed that the transesterification of rapeseed oil with methanol could be catalyzed effectively by basic alkaline earth metal compounds such as calcium oxide, calcium methoxide, and barium hydroxide. Barium hydroxide was the most active catalyst, giving conversions of 75% after 30 min in a batch reactor. Calcium methoxide showed an intermediate activity, and CaO was the least active catalyst nevertheless, 95% conversion could be achieved after 2.5 h in a batch reactor. MgO and Ca(OH)2 showed no catalytic activity for rapeseed oil methanolysis. However, the transesterification reaction rate could be enhanced by the use of ultrasound as well as by introduction of an appropriate co-solvent such as THF to increase methanol solubility in the phase containing the rapeseed oil. [Pg.267]

The rhodium complex [CpRh(bipy)Cl2] is reported (162) to act as one-half of a redox couple that, in concert with a manganese porphyrin system, catalyzes the epoxidation of olefins by dioxygen. In this two-phase system, the aqueous phase contains sodium formate, and the organic phase is a trichloroethane solution of [Mnm(tpp)]1+ and the rhodium complex (tpp = meso-tetraphenylporphyrin). Apparently, the rhodium complex catalyzes the reduction of [Mnin(tpp)]1+ by formate, and the manganese(II) species thus formed binds dioxygen and reacts with the substrate olefin to form the epoxide. However, the intermedi-... [Pg.310]

Numerous dienes can be used as reactants, e.g., isoprene, myrcene, and famesene, and several compounds can be used as active methylene compounds. The reaction proceeds in an aqueous liquid-liquid system, with the conversion regulated by the time of contact between the phases, which is controlled by the stirring. The organic products are easily separated by simple decantation, and the aqueous phase containing the catalyst can be recycled. This reaction was industrialized to produce intermediates for vitamin E such as geranylacetone. The capadty is about 1000 tons/year. [Pg.499]

The representative reaction system applied in asymmetric phase-transfer catalysis is the biphasic system composed of an organic phase containing an acidic methylene or methine compound and an electrophile, and an aqueous or solid phase of inorganic base such as alkaline metal (Na, K, Cs) hydroxide or carbonate. The key reactive intermediate in this type of reaction is the onium carbanion species, mostly onium enolate or nitronate, which reacts with the electrophile in the organic phase to afford the product. [Pg.2]

Annular flow—a liquid film on the walls and a continuous gas phase, containing a mist of liquid droplets, in the core Intermediate slug flow—large gas voids containing liquid droplets Bubble flow—continuous liquid flow with a dispersion of gas bubbles... [Pg.256]

The phase diagrams of two-component surfactant-water systems are typically quite different for nonionic and ionic compounds. As exemplified in Fig. 2.22 there are at low temperatures different liquid crystalline phases while at intermediate temperatures there may be a total mutual solubility of surfactant and water98. At higher temperatures, there is, as already noted, a separation into two phases with a very large two-phase region. One of the phases contains very little surfactant, while the other contains appreciable amounts of both components. The cloud-point curve can be described as a liquid-liquid solubility curve with a lower consolute tempera-... [Pg.27]

Fig. 13 (a, top) Low internal standard responses were observed for incurred samples of some subjects, (b, bottom). Due to variable thickness of intermediate layer between aqueous and organic phases in liquid-liquid extraction, an inappropriately set aspirating height could result in partial transfer of salt-containing intermediate layer, which caused ion suppression. Reproduced from ref. [36] with permission from Elsevier... [Pg.22]

Portland cement clinkers contain small amounts of alkalis and sulphates derived from the raw materials and fuel. Both alkalis and SO3 can be present in the major clinker phases, but tend to combine preferentially with each other to form alkali or potassium calcium sulphates, and it is necessary to consider these components together. In addition, silicate and aluminate phases containing sulphate can form either as intermediates or in undesirable deposits in eement making, and a calcium aluminate sulphate is a major constituent of some expansive and other speeial cements. [Pg.42]

The only phase containing essential alkali but not essential SO3 known to occur in Portland cement clinkers in more than trace amounts is the orthorhombic aluminate phase described in Section 1.4. Trace amounts of alkali carbonates (P2) or potassium aluminate (F4) have been reported to occur in some clinkers, and some other alkali phases are formed as intermediates or deposits. [Pg.54]

The individual hydration products and relevant phase equilibria were described in Chapter 6. The major initial products arc CAHjg at low temperatures, CjAHg and AH, at intermediate temperatures and CjAH, and AH, at higher temperatures (Fig. 10.1). With the passage of time, the other products are replaced by C,AH(, and AH, at rates that depend on the temperature and other factors this process is called conversion. An amorphous or gel phase containing Ca has been reported to form simultaneously with the crystalline products, in a proportion relative to the latter that increases with temperature (E5,E6). [Pg.320]

Little has been published about heat transfer in narrow channels. Some attempts have been made to model heat transfer for segmented flow in small tubes (not capillaries) by Hughmark [28] and Oliver and Young Hoon [29,30]. The concept adopted by these authors is that heat transfer in a two-phase system may be approximated by heat transfer to a single fluid (the liquid phase) contained in a series of shorter tubes with some form of intermediate mixing. However, these studies have been carried out for larger tubes (2.54-cm ID) in which turbulent flow also occurs. Thus, they are not directly applicable to heat transfer monoliths. [Pg.280]

The nucleus is bound by a double-membrane, which is contiguous through the nuclear pores, known as the nuclear envelope. The pores are required to allow RNA out and membrane lipids in (which is needed for growth during S phase). The inner face of the inner nuclear envelope (INE) is coated by the nuclear lamina, which contains intermediate fibres called lamins A, B and C (atleast in mammals). Phosphorylation of lamins by kinases cause nuclear envelope breakdown during prometaphase. Chromosomes occupy definite positions within the nucleus because of the interaction between lamins and telomeres, for example the Rabl conformation in yeast. [Pg.13]


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Intermediate phases

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