Quartz reactors

A solution of 500 mg 3 -acetoxypregn-5-en-20-one-[17a,16a-c]-A -pyrazoline in 100 ml of anhydrous dioxane is stirred with a magnetic stirrer and irradiated in a water-cooled quartz reactor with a high pressure Biosol Philips 250 W quartz lamp for 1 hr. The solvent is removed at reduced pressure and the residue is chromatographed on alumina (activity III). Elution with petroleum ether-benzene (3 1) gives 0.2 g (42%) of 3 -acetoxy-16a,17a-methylene-pregn-5-en-20-one mp 193-193.5° after two recrystallizations from methylene dichloride-ethyl acetate. 

Considering the formation of saturated five-membered heterocycles with two heteroatoms, it is worth to note the possibility to prepare 1,3-dioxolanes, dithiane, oxathianes 148 [93] and dioxolanones 149 [94] by condensation of the corresponding carbonyl compounds under microwave irradiation in acid medium (Scheme 52). The reaction, which is very useful for the protection of carbonyl compounds or for the preparation of useful synthetic intermediates, has also been carried out under batch conditions over Montmorillonite KIO clay in more than 150 g scale, using a 1 L quartz reactor [95]. 

XPS Analysis. The ultrahigh vacuum (OHV) catalyst treatment-surface analysis system employed to characterize and treat the cobalt catalysts has been described previously ( 1, 2 The catalyst treatment and data analysis procedures have also been described (JJ. Briefly, the samples were treated in quartz reactors and then transferred under UHV into a modified Hewlett-Packard 5950A BSCA spectrometer for emalysis. Peak areas were normalized with theoretical cross-sections (Z) to obtain relative atomic compositions. 

The TPD unit was constructed at the Signal UOP Research Laboratory. It Includes a Carle 111 H gas chromatograph with Pd/Ag hydrogen separator, Leeds Northrup temperature programmer, Bascom-Turner 8000 series recorder with data processing and storage capabilities and a custom designed quartz reactor. 

Figure 6 shows typical results obtained with the plug-flow quartz reactor containing 0.5 g of Sr(lwt%)/La203 catalyst operated in the continuous flow recycle mode. The inlet CH partial pressure was 20 kPa (20% CH in He) at inlet flowrates of 7.1 and 14.3 cm STP/min. A 20% O2 in He mixture was supplied directly, at a flowrate Fog, in the recycle loop via a needle valve placed after the reactor (Fig. 1). The methane conversion was controlled by adjusting Fog, which was kept at appropriately low levels so that the oxygen conversion...

The catalyst prepared above was characterized by X-ray diffraction, X-ray photoelectron and Mdssbauer spectroscopic studies. The catalytic activities were evaluated under atmospheric pressure using a conventional gas-flow system with a fixed-bed quartz reactor. The details of the reaction procedure were described elsewhere [13]. The reaction products were analyzed by an on-line gas chromatography. The mass balances for oxygen and carbon beb een the reactants and the products were checked and both were better than 95%. 

The catalytic reactions to produce CH,- radicals and other products were carried out in the fiised-quartz reactor dqiicted in Figure 1. Approximately 200 mg of catalyst was placed near the exit of the reactor. The reactor was connected via a skimmer to... 

Figure 5.28 Schematic of the experimental set-up. Water/ethylene glycol/SDS reservoir (a) high-pressure liquid pumps (b) catalyst/ substrate HPLC injection valve with 200 pi sample loop (c) hydrogen supply, equipped with mass flow controller (d) micro mixer (e) heating jacket (f) tubular glass or quartz reactor (g) back-pressure regulator (h) [64],...

Experiments were carried out in a U-type quartz reactor. The sample (0.025-0.2 g) was held between plugs of quartz wool and the temperature was monitored through a WET 4000 or Eurotherm 2408 temperature controllers. Reactant gases were fed from mass flow controllers (Brooks 5850TR). 

Temperature programmed reduction (TPR) experiments. TPRs were performed for each material using a quartz reactor tube (4 mm i d ), in which a 100 mg sample was mounted on loosely packed quartz wool. Samples were predried overnight at 120 °C. The sample was heated at 5 °C /min up to 700 °C under 20 mL/min flow of a 2 1 mixture of H2 Ar. 

The experimental system consists of three sections (i) a gas metering section with interconnected 4-port and 6-port valves, (ii) a reactor section including an in-situ diffused reflectance infrared Fourier transform spectroscopy reactor (DRIFTS) connected to tubular quartz reactor, (iii) an effluent gas analysis section including a mass spectrometer or a gas chromatograph (9). 

Catalytic runs were carried out in a U-type quartz reactor, under Temperature Programmed Surface Reaction (TPSR) conditions (GHSV= 45000 h"1). The sample was pre-treated in flowing argon from room temperature (RT) to 500 °C, using a heating rate of 5 °C min"1, and kept at 500 °C for lh. Further details are also given elsewhere [19]. 

Since graphite is a very strong absorber of microwave heating, the temperature must be carefully controlled to avoid melting of the reactor. The use of a quartz reactor is highly preferable. 

Steinfeld et al. [133] demonstrated the technical feasibility of solar decomposition of methane using a reactor with a fluidized bed of catalyst particulates. Experimentation was conducted at the Paul Scherrer Institute (PSI, Switzerland) solar furnace delivering up to 15 kW with a peak concentration ratio of 3500 sun. A quartz reactor (diameter 2 cm) with a fluidized bed of Ni (90%)/Al2O3 catalyst and alumina grains was positioned in the focus of the solar furnace. The direct irradiation of the catalyst provided effective heat transfer to the reaction zone. The temperature was maintained below 577°C to prevent rapid deactivation of the catalyst. The outlet gas composition corresponded to 40% conversion of methane to H2 in a single pass. Concentrated solar radiation was used as a source of high-temperature process heat for the production of hydrogen and filamentous... 

Fig. 30 Changes in the concentrations of acetaldehyde and C02 solely by circulation without irradiation and after subsequent irradiation of UV light at various temperatures. The felt material (0.3 g) was placed at the center of the quartz reactor. The initial concentration of acetaldehyde was 250 ppm.

Fig. 4. Configuration of a ceramic membrane reactor for partial oxidation of methane. The membrane tube, with an outside diameter of about 6.5 mm and a length of up to about 30 cm and a wall thickness of 0.25-1.20 mm, was prepared from an electronic/ionic conductor powder (Sr-Fe-Co-O) by a plastic extrusion technique. The quartz reactor supports the ceramic membrane tube through hot Pyrex seals. A Rh-containing reforming catalyst was located adjacent to the tube (57).

The film that was obtained was very thin and it was not possible to grow thicker films. This result was most probably caused by absorption of the incident radiation by the film formed on the interior of the quartz reactor, thereby blocking the incoming UV light and preventing the activation of the monomer and continous polymerization. The UV absorption of the monomer and of polymer film reside in the same region. Figure 18.5 and 18.6 show the UV absorption spectra of the precursor and the polymer film as deposited on the quartz surface, respectively. 

For catalyst treatments, the sample is transferred into the quartz reactor in vacuo, the reactor isolated, the gas flow commenced, and temperature linearly ramped to the desired value. After the sample has been at temperature for the desired time period, the sample is cooled to room temperature in the gas flow, the gas flow is stopped, and the reactor is evacuated. 

Temperature Programmed Reduction (TPR) Studies. In the TPR studies, a gas mixture of 2% H2 in Ar is passed over powdered samples of the calcined catalysts. The catalysts are held in the middle of a 5-mm diameter, 0.4-m long quartz reactor with... 

The stability of C60 and C70 solutions in vegetable oils has been examined also towards the action of UV light. A C60 solution in linseed oil has been irradiated in a quartz reactor with UV light from a 12 W low-pressure Hg lamp having its main emission at 254 nm under N2. In less than 1 hour irradiation, all the visible part of the electronic spectrum of C60 with bands at about 530 and 600 nm have been bleached. Simultaneously, a growth in absorption intensity as function of the irradiation time has been observed at about 410nm. 

The rate of hydrolysis is slower than the corresponding silicon analog, with hydrolysis occurring only partially. When heated with hydrogen at 1,000°C in a quartz reactor, it is converted into germanium(I) chloride, condensing onto the wall of the reactor ... 

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