Crystallization seed crystals

DIAMOND POWDER CARBON HEATER SOLVENT-CATALYST-GROWING CRYSTAL SEED CRYSTAL... 

C<5Cl402. A fungicide mainly used as a seed protectant. Yellow crystals, m.p. 290" C. 

Boil the mixture gently on a sand-bath for 4 hours and then decant into a conical flask and cool. Seed the cold solution if necessary with a trace of a-methylglucoside. The glucoside separates as colourless crystals. When crystallisation ceases, filter the glucoside at the pump, drain, wash quickly with a small quantity of methanol, and then recrystallise from a minimum of methanol. For this purpose methanol of good quality, but not necessarily anhydrous, should be used. The a-methylglucoside is obtained as colourless crystals, m,p. 165°. Yield, 6-7 g. 

The separation of the solid phase does not occur readily with some liquid mixtures and supercooling is observed. Instead of an arrest in the cooling curve at /, the cooling continues along a continuation of c/ and then rises suddenly to meet the line f g which it subsequently follows (Fig. 1,13, 1, iii). The correct freezing point may be obtained by extrapolation of the two parts of the curve (as shown by the dotted line). To avoid supercooling, a few small crystals of the substance which should separate may be added (the process is called seeding ) these act as nuclei for crystallisation. 

Method 2. Place 0-2 g. of cupric acetate, 10 g. of ammonium nitrate, 21 2 g. of benzoin and 70 ml. of an 80 per cent, by volume acetic acid -water solution in a 250 ml. flask fitted with a reflux condenser. Heat the mixture with occasional shaking (1). When solution occurs, a vigorous evolution of nitrogen is observed. Reflux for 90 minutes, cool the solution, seed the solution with a crystal of benzil (2), and allow to stand for 1 hour. Filter at the pump and keep the mother liquor (3) wash well with water and dry (preferably in an oven at 60°). The resulting benzil has m.p. 94-95° and the m.p. is unaffected by recrystallisation from alcohol or from carbon tetrachloride (2 ml. per gram). Dilution of the mother liquor with the aqueous washings gives a further 1 Og. of benzil (4). 

C,H,CH,- —C-NH,j The compound separates in either, sometimes as both, of two dimorphic forms, m.p. 150° and 175° respectively. The former may be converted into the higher m.p. form by dissolving It in alcohol and seeding with crystals of the form, m.p. 175° the low m.p. form when warmed to 175° gives, after sohdification, a m.p. of 175°. Both dimorphic forms give identical derivatives with carboxyUc acids and sulphonic acids (see Sections 111,85 and IV,33). 

A higher density sol—gel abrasive, produced by the introduction of seed crystaUites formed by wet-milling with high alumina media or by introduction of submicrometer a-alumina particles, was patented (28) and designated Norton SG. The microstmcture of this abrasive consists of submicrometer a-alumina crystals (Fig. 1) and its bulk density approaches that of fused alumina. Norton SG has proven to be an exceptional performer in coated and bonded abrasive products it was awarded the 1989 ASM Engineering Materials Achievement Award (29). 

The softened seawater is fed with dry or slaked lime (dolime) to a reactor. After precipitation in the reactor, a flocculating agent is added and the slurry is pumped to a thickener where the precipitate settles. The spent seawater overflows the thickener and is returned to the sea. A portion of the thickener underflow is recirculated to the reactor to seed crystal growth and improve settling and filtering characteristics of the precipitate. The remainder of the thickener underflow is pumped to a countercurrent washing system. In this system the slurry is washed with freshwater to remove the soluble salts. The washed slurry is vacuum-filtered to produce a filter cake that contains about 50% Mg(OH)2. Typical dimensions for equipment used in the seawater process may be found in the Hterature (75). 

Precipitation. The precipitation of aluminum tribydroxide ia the recovery step of the Bayer process is achieved either by loweting the temperature or by diluting the pregnant Hquor and reduciag its pH. Both methods reverse the direction of equation 35, but seeding with previously precipitated crystals is required ia order to initiate nucleation. 

The concentrated mother Hquor contains a large amount of sulfuric acid in a free form, as titanium oxy-sulfate, and as some metal impurity sulfates. To yield the purest form of hydrated TiOg, the hydrolysis is carried out by a dding crystallizing seeds to the filtrate and heating the mixture close to its boiling temperature, - 109° C. The crystal stmcture of the seeds (anatase or mtile) and their physical properties affect the pigmentary characteristics of the final product. 

During calcination, water is removed at temperatures between 200 and 300°C sulfur trioxide is removed at temperatures between 480 and 800°C. At about 480°C the crystals of Ti02 are being formed and continue to grow with increasing temperature. To prepare the anatase pigment, the final calcination temperature of the hydrolysate prepared in the presence of anatase seeds should reach about 800—850°C. 

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