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1
Content available Method of utilization of the spent vanadium catalyst
EN
A spent vanadium catalyst, from the plant of metallurgical type, was leached in a potassium hydroxide solution to recover vanadium. The effect of time, temperature, concentration of basic, catalyst particle size and phase ratio was studied. The results showed that for a 160–750 μm catalyst leached for 4 h at 313.15 K in the presence of 10% potassium hydroxide solution at a liquid: solid ratio of 20:1, the extent of leaching of V was about 87%. Additionally, separation of vanadium from such a solution was investigated by the ion exchange method. Two types of polymer strongly basic ion exchangers were used. The ion exchange tests indicate that vanadium were loaded from the post-leaching solution with high efficiency. On this basis a flowsheet for the proposed process of a complex utilization of the spent vanadium catalyst is presented.
PL
Przedstawiono wyniki badań otrzymywania węglanu wapnia z płynu podestylacyjnego DS i nasyconego roztworu wodorowęglanu sodu z metody Solvaya w obecności wersenianu disodu. Badania prowadzono w temp. 20, 50 i 90°C. Roztwory dozowano w stosunku stechiometrycznym, stosując szybkości dozowania 23,6 oraz 95 cm3/min. Stosowano wersenian disodu o stężeniu 1 i 10 g/dm3 płynu DS. Dla otrzymanych prób CaCO3 oznaczano gęstość nasypową i utrząsową, chłonność wody, oleju parafinowego i ftalanu dibutylu, oraz formę krystalograficzną otrzymanych kryształów.
EN
CaCO3 was pptd. from the waste distn. liq. from Solvay process by addn. of satd. soln. of NaHCO3 in a lab. reactor at 20–90°C and varying dosing rate in presence of Na2 versenate and studied for bulk and packing d., cryst. structure and H2O, paraffinic oil and Bu2 phthalate absorption capacity. The addn. of Na2 versenate at 90°C resulted in an increase in the d. of CaCO3 crystals. At 90°C, the calcite and aragonite crystals were formed. At lower temps., formation of calcite crystals was also obsd.
EN
The results of the precipitation of calcium carbonate from a waste post-distillation liquid (DS) and a sodium bicarbonate saturated solution – both from the Solvay method – in the presence of urea are presented. The investigation was carried out at 293 K and 343 K. Reagent dosage times of 1, 5, 10, 20 and 30 min, and urea concentrations of 5, 6 and 10 mol/dm3 were applied. The granulometric composition, the values of bulk and packing densities and the absorptiveness sorption of water and paraffin oil from the obtained calcium carbonate were investigated.
EN
The results of the leaching of vanadium(V) from the mixture after potassium metavanadate synthesis from KCl and spent vanadium catalyst in the presence of steam were presented. Spent vanadium catalyst was obtained from the waste storage of a chemical plant producing sulfuric acid(VI) by the contact method. The reaction mixture was leached using different solutions: 1 M Na2CO3, 20% CO(NH2)2, 15% NaOH, 15% KOH, 2 M H2SO4. The effect of time and temperature was studied. The results showed that for reaction mixture leached for 4 h at 303 K in the presence of 15% sodium hydroxide solution at a liquid:solid ratio of 10:1, the extent of leaching of vanadium(V) was 95.43%.
EN
The optimal conditions were determined for the precipitation of ammonium metavanadate from the solutions of ammonium nitrate with the use of sodium metavanadate. The experiments were performed with the molar ratio of salts NH4NO3:NaVO3 1.5:1 at temperatures 293, 303, 313 and 323 K. Based on the obtained results, the optimal time of the process was determined as 5 h at 293–303K. Under these conditions, the achieved yield of the precipitation process was ~98.7%, while the contents of the vanadium salts in the post – filtration solution was ~0.02%.
EN
Investigation was carried out on the optimal conditions of the synthesis of NaVO3 and Cl2 from NaCl and V2O5 in the presence of the atmospheric oxygen. The influence of the excess of NaCl relative to V2O5 was investigated. Also the effect of the quartz sand introduced into the reaction mixture on the yield of the NaVO3 synthesis was determined. The obtained product of synthesis was isolated from the post-reaction mixture.
EN
The influence of urea on the vanadium(V) and potassium ion concentrations in the K2CO3 + NH4VO3 + H2O system was determined in the temperature range of 293 K to 313 K. Additionally, the solution density dependence versus the urea concentration was presented. These data are essential for the assessment of optimum operating conditions for the new production process of potassium carbonate.
EN
The results of the precipitation of calcium carbonate from waste distillation liquor (DS) from the Solvay method and sodium bicarbonate saturated solution in the presence of urea were presented. The investigation was carried out at 293K. The influence of the time of reagents dosage to the solution of urea on the physicochemical character of obtaining product was studied. The time of reagents dosage: 1, 5, 10, 20, 30 min and the concentration of the urea applied: 0.5, 1, 2 and 4 mol/dm3. The granulometric composition, the values of bulk and packing densities and the absorptiveness sorption of water and paraffin oil of the obtaining calcium carbonate were investigated.
13
Content available remote Solubility in the KVO[3] + NH[3] + CO[2] + H[2]O system from 293K to 303K
EN
Solubility in the KVO[3] + NH[3] + CO[2] + H[2]O system and the saturated solution densities were measured employing the isothermal solution saturation method. Investigations in the given range of the NH3 concentration varying from 0.1 to 0.6 mol[x]dm[^-3], as a function of time and temperature, have been carried out. The data presented herein is essential for the assessment of optimum operating conditions for the production process of potassium carbonate introducing the modified Solvay's method.
PL
Metodą izotermicznego nasycania roztworów zbadano rozpuszczalność i oznaczono gęstość roztworów równowagowych w układzie KVO[3] + NH[3] + CO[2] + H[2]O. Badania prowadzono w zakresie stężeń NH3 od 0,1 to 0,6 mol[x]dm[^-3], w zależnośvi od czasu i temperatury. Uzyskane dane są niezbędne przy opracowaniu optymalnych parametrów otrzymywania węglanu potasu zmodyfikowaną metodą Solvaya.
EN
The research was conducted to determine the influence of the urea concentration in the leaching solutions on the efficiency of recovery of vanadium and iron compounds from the used vanadium catalyst from the node of oxidation of sulfur dioxide to sulfur trioxide.
EN
The mutual solubility of salts in the NaVO3-NaNO3-H2O system was investigated at 293 - 323 K temperature range by the method of isothermal saturation of solutions. A fragment of the solubility polytherm for that system was plotted, based on the obtained data. The investigated system is a part of the quaternary NH4NO3-NaVO3-NH4VO3-NaNO3 system, and it is necessary for plotting the solubility isotherm as a planar projection according to Janecke, since it defines one edge of its square. Knowledge of the isotherm for that quaternary system is necessary to determine the optimal utilization conditions for the post-filtration lye, formed during the soda production from NaNO3 by the Solvay method, using NaVO3.
EN
The influence of urea on the vanadium(V) and potassium ion concentrations in the KHCO3 + NH4VO3 + H2O system was determined in the temperature range of 293 K to 303 K. Additionally, the solution density dependence versus the urea concentration was presented. These data are essential for the assessment of optimum operating conditions for the new production process of potassium carbonate.
PL
Podjęto badania dotyczące wykorzystania zużytego katalizatora wanadowego do syntezy metawanadanu(V) sodu z NaCl oraz metawanadanu(V) potasu z KCl, prowadzonej przy współudziale tlenu z powietrza.
EN
At 873 K, reactions 4(Na or K)Cl + 2V2O5 (spent catalyst) + O2 = 4(Na or K)VO3 + 2Cl2 gave (Na or K)VO3 in (87% or 26%) yields in 4 hrs, air flow rate 182 cm3/min, and with NaCl used in 15% and KCl in 50% excess over V2O5. The catalyst calcined at 800°C/21 hrs. was free of S oxides. The catalyst particle size fractions 0.090–0.125 and 0.355–0.5 mm were resp. best to get the above max. yields
PL
Metodą izotermicznego nasycania roztworów zbadano wpływ stężenia wodorowęglanu potasu na rozpuszczalność metawanadanu(V) amonu w wodzie w temperaturach 313 i 323 K. Uzyskane wyniki stanowiły podstawę do wykreślenia izoterm rozpuszczalności układu KHCO3– NH4VO3–H2O oraz określenia wpływu temperatury i stężenia NH4VO3 na zmiany gęstości badanych roztworów równowagowych. Prezentowane dane są niezbędne przy opracowaniu niskoodpadowej metody wytwarzania K2CO3 w oparciu o karbonizację wodno-amoniakalnych roztworów KVO3.
EN
The soly. of NH4VO3 in aq. solns. was studied by isothermal satn. technique at 313 and 323 K. Soly. isotherms were detd. in the KHCO3–NH4VO3–H2O system and the d. of equil. solns was examd. in relation to NH4VO3 concn. and temp. The data are essential for developing a low-waste prepn. of K2CO3 by carbonation of aq.-ammoniacal KVO3 solns. Solid phases at equil. were identified by X-ray diffraction / were x-rayed. In satd.KHCO3, NH4VO3 affected only slightly the soly of KHCO3. The KHCO3 salted-in NH4VO3 considerably. As temp. was raised, the solys. of KHCO3 and NH4VO3 rose. The d. of satd. KHCO3 rose to attain max. at the temp.-invariant (eutonic) p., then fell to the ds. corresponding to satd. NH4VO3 solns. At each temp., KHCO3 and NH4VO3 were the solids at equil. with the soln. along the lower and the upper boundaries, resp.
19
Content available remote Otrzymywanie węglanu wapnia o niskiej gęstości utrząsowej
PL
Zaprezentowano wyniki badań otrzymywania węglanu wapnia z odpadowego płynu podestylacyjnego DS oraz nasyconego roztworu wodorowęglanu sodu z wykorzystaniem wodnych roztworów mocznika. Badania prowadzono w temp. 333 K. W otrzymanych próbach węglanu wapnia oznaczano gęstość nasypową i utrząsową, punkt płynięcia oraz rodzaj kryształów.
EN
CaCO3 was pptd. in aq. 0.5–2 M urea by using Solvay’s aq. satd. NaHCO3 and waste distn residue (NH3 recovery step) at 333 K. Bulk and tap ds., flow p., and habitus of CaCO3 were detd. The residue was aq. CaCl2 and NaCl with solids and SO4 as impurities which were removed by clearing and filtration. The NaHCO3 soln. was prepd. from crude NaHCO3 taken from the filtration step. The longer the reactants dosing time, the higher the bulk and tap ds. and the lower the CaCO3 flow p. The higher the urea concn., the lower the tap d. (min. at 606 g/l. in 2 M urea), regardless of the dosing time. Urea made the calcite type to cryst., yet conglomerate was the most frequent habitus type.
PL
Przeprowadzono badania określające możliwość wykorzystania rozcieńczonych roztworów mocznika do odzyskiwania związków wanadu(V) ze zużytego katalizatora wanadowego. Oszacowano wpływ czasu i temperatury na wydajność procesu ługowania.
EN
The spent catalyst, 5.0 g, was treated with 50 ml aq. 20% urea at 295–320 K for 5–120 min and filtered. The filtrate was analyzed for V(V) and the max. recovered concn. was 0.0195 mol V/l. Temp. was a minor factor and time was significant for the first 30 min.
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