Solvent powder

The fusion of powdered potassium hydroxide and carbazole together at 220-260°C has been often used for the preparation of the potassium salt of carbazole, the salt then being utilized in hydrocarbon solvent powdered potassium hydroxide was shown " to be better for this purpose than strong aqueous sodium hydroxide. Many 9-alkylations have been conducted in this way including preparations of dicarbazol-9-ylalkanes [29 R = (CH2)3 g-carbazol-9-yl] (using the corresponding dihalides), 9-(2,3-epoxyprop-l-yl) O / ... 

BIOS/JAP/PR/1292/Report. Japanese Propellants—Research on Non-volatile Solvent Powders, H.M.S.O., London. 

A new electrically conductive gjove made of "Velostat is said id be the solution for use during static hazardous operations. The gloves drain off static charges when the wearer is grounded. Chemically resistant, they are claimed to provide protection from acids, alkalies, and other contaminants that can cause injury. Manufacturer especially recommends disposable gloves for those working with flammable solvents, powders, liquids, and dusts... 

Physical properties of cast propellants German cast propellants for rockets General safety considerations in the manufacture of smokeless powder Solvents Powder grains Building and their lay out Literature... 

The yV-alkyl-substituted azadiol was treated with an equimolar amount of tosyl chloride and excess alkali metal hydroxide in an aprotic solvent (powdered NaOH, dioxane, room temperature, 3 hr) to give a 60% yield of the monoaza-crown (Kuo et al., 1978). Template effects are important in this cyclization reaction, so sodium hydroxide was used for aza-15-crown-5 and potassium hydroxide for aza-18-crown-6. The intramolecular ring-closure process is the result of the initial formation of a tosylate by the reaction of one alkoxide anion with tosyl chloride followed by displacement of the tosylate leaving group by the second alkoxide anion. The pure monoaza-crowns were isolated from their metal ion complexes by thermolysis under reduced pressure (Kuo et al., 1980). 

Solvent Powder. See under Single-Base and Double-Base Cannon Propellants in Vol 2, C31-R to C33-R, and Production Methods of Representative Propellants in Vol 8, P420-L... 

Solvent-free products. The products of fliis group are produced and applied without organic solvents powder coatings, radiation curing systems, solvent-free water coating (without cosolvents). 

In spite of the development of environmentally friendly coating systems, based on the use of low-solvent content paints, free-solvent powder coatings, and waterbome-based products, many of the traditional organic solvent-based paints are difficult to replace without affecting the quality of the finished products. 

Fluorocarbon Solvent, powder Bake Hi iest exterior durability, chemical resistance Adhesion, recoatability, high baking temperatures High Coil (xmtings, siding... 

Vinyl Solvent, powder (a) Must be modified with other resins Air dry, bake Chemical resistance, flexibility, fast air dry, fon ility, resistance to acid, alkali, abrasion Generally low solids, low flash pmnts Modnate Can and tank linings, maintenance mints, metal decorating paints... 

XRD diffraction studies was also carried out to analyze the crystallinity of the polymers 3(a-d) and was performed at room temperature. To avoid the trace of the solvents, powder samples were placed on a zero-background quartz plate, placed for 20 s. in an oven preheated to 110 °C, quenched to room temperature using a N2 purge, and then analyzed in the diffractometer. The XRD patterns are shown in Fig. 12.6. All the polymers show similar multiple sharp diffraction peaks in the range of 20 = 11.0°-30.0° which indicates the crystalline to semi-crystalline nature of the polymers. This may be due to the slight difference in the chemical structures of these polymers. Furthermore, the results of the x-ray diffraction were in agreement with the POM textures, and this confirmed that the synthesized polymers 3(b-d) were in liquid crystal phases (nematic mesophase). 

Cubic BN powders (usually < 0.5 mm in size) are produced when hBN powders mixed with solvent powders are subjected to pressure > 5 GPa and temperatures > 1500°C for several minutes. Commercial cBN powders are mass produced in this way. For diamond synthesis by the high-pressure film method, described in Sec. IV.A.1, a thin solvent film always exists between the graphite source material and the diamond crystal produced. The formation mechanism of cBN powders is believed to be the same as that for the synthesis of diamond by the high-pressure film method, although a solvent film between the hBN source material and the cBN crystal produced has not been observed as clearly as it has been for diamond (223). 

In the commercial extraction of alkaloids from the drugs in which they exist, the powdered drug, or an alcoholic extract of it, is treated with an alkali such as ammonia or lime to liberate the alkaloid and the alkaloid is then extracted by means of an organic solvent. The crude material thus obtained is purified and finally crystallized either as the base itself or as its water-soluble salts. 

For tire purjDoses of tliis review, a nanocrystal is defined as a crystalline solid, witli feature sizes less tlian 50 nm, recovered as a purified powder from a chemical syntliesis and subsequently dissolved as isolated particles in an appropriate solvent. In many ways, tliis definition shares many features witli tliat of colloids , defined broadly as a particle tliat has some linear dimension between 1 and 1000 nm [1] tire study of nanocrystals may be drought of as a new kind of colloid science [2]. Much of die early work on colloidal metal and semiconductor particles stemmed from die photophysics and applications to electrochemistry. (See, for example, die excellent review by Henglein [3].) However, the definition of a colloid does not include any specification of die internal stmcture of die particle. Therein lies die cmcial distinction in nanocrystals, die interior crystalline stmcture is of overwhelming importance. Nanocrystals must tmly be little solids (figure C2.17.1), widi internal stmctures equivalent (or nearly equivalent) to drat of bulk materials. This is a necessary condition if size-dependent studies of nanometre-sized objects are to offer any insight into die behaviour of bulk solids. 

Wlrile size distribution is important, control over tire nanocrystal surface is equally important. The best nanocrystal syntlieses provide avenues for nanocrystals to be purified, collected as powders, and tlien redissolved in appropriate solvents. This requires control over tire surface chemistry, in order to control tire solubility of tire nanocrystals. 

Decolorisation by Animal Charcoal. It sometimes hap pens (particularly with aromatic and heterocyclic compounds) that a crude product may contain a coloured impurity, which on recrystallisation dissolves in the boiling solvent, but is then partly occluded by crystals as they form and grow in the cooling solution. Sometimes a very tenacious occlusion may thus occur, and repeated and very wasteful recrystallisation may be necessary to eliminate the impurity. Moreover, the amount of the impurity present may be so small that the melting-point and analytical values of the compound are not sensibly affected, yet the appearance of the sample is ruined. Such impurities can usually be readily removed by boiling the substance in solution with a small quantity of finely powdered animal charcoal for a short time, and then filtering the solution while hot. The animal charcoal adsorbs the coloured impurity, and the filtrate is usually almost free from extraneous colour and deposits therefore pure crystals. This decolorisation by animal charcoal occurs most readily in aqueous solution, but can be performed in almost any organic solvent. Care should be taken not to use an excessive quantity... 

A) Extract the mixture with about 40 ml. of chloroform, in which the free base is very soluble. Run off the lower chloroform layer, dry it with potassium carbonate as in (a), and then add carbon tetrachloride slowly with stirring to the filtered chloroform solution until the base starts to crystallise out. Allow to stand for a short time (t.e., until the deposition of crystals ceases) and then filter at the pump as the crystals lose the last trace of solvent, they tend as before to break up into a fine powder, the deep green colour becoming paler in consequence. 

Although benzenesulphonyl chloride has for simplicity been used in the above discussion, tolucne-/>- sulphonyl chloride, CHaCeH SO Cl, is more frequently used in the laboratory, owing to its much lower cost, the latter being due in turn to the fact that toluene-p-sulphonyl chloride is a by-product in the commercial preparation of saccharin. Toluene-p sulphonyl chloride is a crystalline substance, of m.p. 68° the finely powdered chloride will, however, usually react readily with amines in the Schotten-Baumann reaction it does not react so readily with alcohols, but the reaction may be promoted considerably by first dissolving the chloride in some inert water-soluble solvent such as acetone. 

Bromoform. Commercial bromoform should be shaken thoroughly with water, separated, dried over powdered anhydrous sodium sulphate and then fractionally distilled under reduced pressure using a water-condenser. It should be stored in a dark cupboard. It is an excellent solvent, has the advantage of a high Constant, and very seldom causes association of the solute. 

The choice of solvent cannot usually be made on the basis of theoretical considerations alone (see below), but must be experimentally determined, if no information is already available. About 0 -1 g. of the powdered substance is placed in a small test-tube (75 X 11 or 110 X 12 mm.) and the solvent is added a drop at a time (best with a calibrated dropper. Fig. 11, 27, 1) with continuous shaking of the test-tube. After about 1 ml. of the solvent has been added, the mixture is heated to boiling, due precautions being taken if the solvent is inflammable. If the sample dissolves easily in 1 ml. of cold solvent or upon gentle warming, the solvent is unsuitable. If aU the solid does not dissolve, more 11,27,1. solvent is added in 0-5 ml. portions, and again heated to boiling after each addition. If 3 ml. of solvent is added and the substance... 

Add 1 ml. of the alcohol-free ether to 0-1-0-15 g. of finely-powdered anhydrous zinc chloride and 0 5 g. of pure 3 5-dinitrobenzoyl chloride (Section 111,27,1) contained in a test-tube attach a small water condenser and reflux gently for 1 hour. Treat the reaction product with 10 ml. of 1-5N sodium carbonate solution, heat and stir the mixture for 1 minute upon a boiling water bath, allow to cool, and filter at the pump. Wash the precipitate with 5 ml. of 1 5N sodium carbonate solution and twice with 6 ml. of ether. Dry on a porous tile or upon a pad of filter paper. Transfer the crude ester to a test-tube and boil it with 10 ml. of chloroform or carbon tetrachloride filter the hot solution, if necessary. If the ester does not separate on cooling, evaporate to dryness on a water bath, and recrystallise the residue from 2-3 ml. of either of the above solvents. Determine the melting point of the resulting 3 5 dinitro benzoate (Section 111,27). 

Suspend in a round-bottomed flask 1 g. of the substance in 75-80 ml. of boihng water to which about 0 -5 g. of sodium carbonate crystals have been added, and introduce slowly 4 g. of finely-powdered potassium permanganate. Heat under reflux until the purple colour of the permanganate has disappeared (1-4 hours). Allow the mixture to cool and carefully acidify with dilute sulphuric acid. Heat the mixture under reflux for a further 30 minutes and then cool. Remove any excess of manganese dioxide by the addition of a little sodium bisulphite. Filter the precipitated acid and recrystallise it from a suitable solvent (e.g., benzene, alcohol, dilute alcohol or water). If the acid does not separate from the solution, extract it with ether, benzene or carbon tetrachloride. 

The experimental conditions for conducting the above reaction in the presence of dimethylformamide as a solvent are as follows. In a 250 ml. three-necked flask, equipped with a reflux condenser and a tantalum wire Hershberg-type stirrer, place 20 g. of o-chloronitrobenzene and 100 ml. of diinethylform-amide (dried over anhydrous calcium sulphate). Heat the solution to reflux and add 20 g. of activated copper bronze in one portion. Heat under reflux for 4 hours, add another 20 g. portion of copper powder, and continue refluxing for a second 4-hour period. Allow to cool, pour the reaction mixture into 2 litres of water, and filter with suction. Extract the solids with three 200 ml. portions of boiling ethanol alternatively, use 300 ml. of ethanol in a Soxhlet apparatus. Isolate the 2 2- dinitrodiphenyl from the alcoholic extracts as described above the 3ueld of product, m.p. 124-125°, is 11 - 5 g. 

Benzylatnine. Warm an alcoholic suspension of 118-5 g. of finely-powdered benzyl phthalimide with 25 g. of 100 per cent, hydrazine hydrate (CAUTION corrosive liquid) a white, gelatinous precipitate is produced rapidly. Decompose the latter (when its formation appears complete) by heating with excess of hydrochloric acid on a steam bath. Collect the phthalyl hydrazide which separates by suction filtration, and wash it with a little water. Concentrate the filtrate by distillation to remove alcohol, cool, filter from the small amount of precipitated phthalyl hydrazide, render alkaline with excess of sodium hydroxide solution, and extract the liberated benzylamine with ether. Dry the ethereal solution with potassium hydroxide pellets, remove the solvent (compare Fig. //, 13, 4) on a water bath and finally distil the residue. Collect the benzylamine at 185-187° the 3ueld is 50 g. 

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