Silica, filtration

The explosive properties of liquid methane-oxygen mixtures were determined [8], Dining investigation of an explosion in a portable air liquefaction-separation plant, hydrocarbon oil was found in a silica filtration bed [9], The mechanism of slow heterogeneous accumulation of hydrocarbons dissolved in trace amounts in liquid oxygen on the liquid evaporator surfaces is discussed. It was concluded that months of continuous evaporation would be required to attain explosion-hazardous levels in real evaporators [10],... 

The separation of particles of different sizes, and the preparation of colloids of uniform particle size, can be effected by the method of ultrafiltration, depending on the use of filter paper which has been soaked in collodion solution and then immersed in water, or soaked in gelatin solution and then immersed in formaldehyde solution, or gelatinous silica, filtration being done under pressure. By examining the diffusibility of dyes through parchment... 

With Stirring, hydrazine hydrate (4 ml in 30 ml of THh ) was added over 60 min. The reaction mixture was then cooled to room temperature and filtered through Celite. The filtrate was concentrated in vacuo and the residue purified by chromatography through silica gel using 10% ether in hexane for elution. The fractions containing product were combined and evaporated to give the product as a clear oil (2.94g, 50%). 

A mixture of l-(r-Boc)indol-2-yl-tri- -butylstannanc (1.2 mmol) and 4-bromo-benzonitrile (1.0 mmol) and Pd(PPh3)2C , (0.02 mmol) in dry dioxane (5 ml) was heated at I00°C overnight under nitrogen. The reaction mixture was cooled, diluted with EtOAc and stirred for 15 min with 15% aq. KF. The precipitate was removed by filtration and washed with EtOAc. The EtOAc layer was separated, washed with brine, dried (Na2S04) and concentrated. The residue was purified by chromatography on silica. The yield was 66%. 

The reactions of oxiranes with thiocyanate ion or with thiourea are usually done in homogeneous solution in water, alcohols or alcohol-acetic acid. The use of silica gel as a support for potassium thiocyanate in toluene solvent is advantageous for the simple work-up (filtration and evaporation of solvent) (80JOC4254). A crown ether has been used to catalyze reactions of potassium thiocyanate. 

Filter aids should have low bulk density to minimize settling and aid good distribution on a filter-medium surface that may not be horizontal. They should also be porous and capable of forming a porous cake to minimize flow resistance, and they must be chemically inert to the filtrate. These characteristics are all found in the two most popular commercial filter aids diatomaceous silica (also called diatomite, or diatomaceous earth), which is an almost pure silica prepared from deposits of diatom skeletons and expanded perhte, particles of puffed lava that are principally aluminum alkali siheate. Cellulosic fibers (ground wood pulp) are sometimes used when siliceous materials cannot be used but are much more compressible. The use of other less effective aids (e.g., carbon and gypsum) may be justified in special cases. Sometimes a combination or carbon and diatomaceous silica permits adsorption in addition to filter-aid performance. Various other materials, such as salt, fine sand, starch, and precipitated calcium carbonate, are employed in specific industries where they represent either waste material or inexpensive alternatives to conventional filter aids. 

General procedure. LaNIs ingot (3 g) in an autoclave was evacuated at 0.1 mm, heated to 200°C under Hz at 30 atm for 10 min. After cooling to 20°C, Itie operation was repeated five times. The autoclave was cooled in dry ice-acetone, Hg was released and Ng was Introduced. The organic compound (1 mmol) m THFJ4eOH (2 1) (5 mL) was added at -78°C with stirring. Tt mixture was stirred under Ng at 0°C and then at 20°C. The catalyst was filtered, the filtrate concentrated and the residue purified by preparative TLC on silica gel. 

Carbon soot from resistive heating of a carbon rod in a partial helium atmosphere (0.3bar) under specified conditions is extracted with boiling C H or toluene, filtered and the red-brown soln evapd to give crystalline material in 14% yield which is mainly a mixture of fullerenes C q and C70. Chromatographic filtration of the crude mixture with allows no separation of components, but some separation was observed on silica gel... 

A soft, gritty amorphous silica composed of minute siliceous skeletons of small aquatic plants. Used in filtration and decoloration of liquids, insulation, filler in dynamite, wax, textiles, plastics, paint, and rubber. Calcined and flux-calcined diatomaceous earth contains appreciable amounts of cristobalite, and dust levels should be the same as for cristobalite. 

Diatomaceous earth, widely-known and long-used as a filteraid in process and waste filtrations, has a high microcrystalline silica content. As well as being a respiratory hazard in the workplace, the silica is being scrutinized in some jurisdictions as a potentially hazardous dust in landfills in which spent filter cakes are deposited. 

Coal (hard) and coke are used in water filtration, primarily for the removal of coarse suspensions, care being taken to prevent them from scouring or washing away, because of their relative lighmess and fine division. Coal is principally composed of carbon, and is inert to acids and alkalies. Its irregular shapes are advantageous at times over silica sand. 

Coagulation involves the addition of chemicals to alter the physical state of dissolved and suspended solids. This facilitates their removal by sedimentation and filtration. The most common primary coagulants are alum ferric sulfate and ferric chloride. Additional chemicals that may be added to enhance coagulation include activate silica, a complex silicate made from sodium silicate, and charged organic molecules called polyelectrolytes, which include large-molecular-weight polyacrylamides, dimethyl-diallylammonium chloride, polyamines, and starch. 

The size separation of proteins has been routinely called gel filtration because of the historic use of cross-linked gels for this application. Specially modified Zorbax PSM columns, Zorbax GF-250 and Zorbax GE-450, are used for separating proteins by size. These columns are packed with porous silica micro-... 

I. SILICA-BASED TSK-GEL SW/SWxl COLUMNS FOR GEL-FILTRATION CHROMATOGRAPHY (GFC)... 

Boil the tartaric acid and caustic soda solution for three hours in a round flask (I litre), or preferably in a tin bottle furnished with reflu. condenser. The use of a tin vessel obviates certain clitli-cultiesof filtration which the solution of the silica by the action of the alkali on the glass entails. The liquid, after boilinjg, is carefully neutralised with cone, hydrochloric acid (it is acl is-able to remove a little of the solution beforehand in case overshooting the mark) and an excess of calcium chloride solution is added to the hot liquid. The mixture is left overni hl. and the calcium salts filtered off at the pump, washed with water, and well pressed. 

To a solution of m-ethyl cinnamate (44, 352 mg, 85% pure, 1.70 mmol) and 4-phenylpyridine-A-oxide (85.5 mg, 29 mol%) in 1,2-dichloromethane (4.0 mL) was added catalyst 12 (38.0 mg, 3.5 mol%). The resulting brown solution was cooled to 4°C and then combined with 4.0 mL (8.9 mmol) of pre-cooled bleach solution. The two-phase mixture was stirred for 12 h at 4°C. The reaction mixture was diluted with methyl-t-butyl ether (40 mL) and the organic phase separated, washed with water (2 x 40 mL), brine (40 mL), and then dried over Na2S04. The drying agent was removed by filtration the mother liquors concentrated under reduce pressure. The resulting residue was purified by flash chromatography (silica gel, pet ether/ether = 87 13 v/v) to afford a fraction enriched in cis-epoxide (45, cis/trans . 96 4, 215 mg) and a fraction enriched in trans-epoxide cis/trans 13 87, 54 mg). The combined yield of pure epoxides was 83%. ee of the cis-epoxide was determined to be 92% and the trans-epoxide to be 65%. 

B. Methyl indole-4-carboxylate (30). A mixture of 7.0 g (28 mmol) of methyl trans-2-[ -(dimethylamino)vinyl]-3-nitrobenzoate(29) in 140 mL of dry benzene which contained 1.4 g of 10% Pd/C was shaken in a Parr apparatus under Hj (50 psi) for 1.5 h. The catalyst was removed by filtration, and the benzene solution was washed with 30 mL of 5% aq. HCl, brine and dried over MgS04. After removal of the solvent under reduced pressure, the residue was purified via chromatography on silica gel to furnish 6.9 g (82%) of methyl indole-4-carboxylate (30). 

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