Antimony sulfide, preparation

SpiessglanZ kermes, m. kermesite kermes mineral, -kbnig, m. regulus of antimony, -leber,/. livex of antimony, hepar antimonii. -metall, n. antimony, -mittel, n. antimonial remedy, -mohr, m. aethiops antimonialis (old pharmaceutical preparation of mercury and antimony sulfides). -ocker, m, antimony ocher, -oxyd,n. antimon> trioxide. -safran,... 

Under severe initiation conditions, ammonium perchlorate can be made to explode by itself [10]. Mixtures of ammonium perchlorate with sulfur and antimony sulfide are reported to be considerably more shock sensitive than comparable KCIO 3 compositions [2]. Ammonium perchlorate can be used to produce excellent colors, with little solid residue, but care must be exercised at all times with this oxidizer. The explosive properties of this material suggest that minimum amounts of bulk composition should be prepared at one time, and large quantities should not be stored at manufacturing sites. 

The standard American flash and sound composition is a blend of potassium perchlorate, sulfur or antimony sulfide, and aluminum. The ignition temperature of this formulation is several hundred degrees higher than chlorate-based mixtures, but these are still very dangerous compositions because of their extreme sensitivity to spark and flame. Ignition of a small portion of a "flash and sound" mixture will rapidly propagate through the entire sample. These mixtures should only be prepared remotely, by experienced personnel. Table 8.5 hsts several "flash and sound" formulas. 

Into a porcelain dish, place 70 gram of potassium chlorate, 70 grams of freshly prepared wet mercury fulminate, 60 grams of antimony sulfide, and then 10 grams of styphnic acid. Then manual blend this mixture for several hours. A mixing drum may... 

Common Related Antimony Compounds Within the antimony compounds, there are antimony hydride (SbHj, stibine, a gas) which is the most deadly compound, followed by antimony sulfide (Sb2S3, stibi), which is used as a medicament for skin complains and burns. Antimony sulfites are used in rubber compounding, and in camouflage paints because of its reflection of infrared. An antimony salt of tartaric acid, known as tartar emetic, is prepared by leaving some wine in a cup made of antimony overnight (this compound was then used by vets and doctors, mainly to expel bad humours from the body). 

Li the nineteenth century, several investigators [11-13] prepared metathioantimonides by saturating aqUeous solutions of metal sulfides or hydroxides with antimony sulfide or by fusing SbSj with alkali carbonates. However, in most cases, they were unable to separate these compounds. 

Sources such as Riffault et al. (1874) and Heaton (1928) also describe the composition of an antimony vermilion (presumably the same as antimony red mentioned in other sources) as a red form of antimony sulfide. This generally seems to be prepared by precipitation from the chloride - for example, Gettens and Stout (1966) state that synthesis is by precipitating antimony chloride with sodium thiosulfate or widi hydrogen sulfide. It was apparently introduced as a pigment by Murdoch in 1847. 

Riffault et al. (1874) describe a while anlimoniale of lead , the preparation being to mix one part antimony sulfide (stibnite,. v.) with five parts potassium nitrate, this being heated to red hot the product is dissolved in water and a neutral lead acetate solution added. Essentially the same recipe occurs in the text by Bersch (1901), who describes this and lead antimonite as heavy, white powder... dearer than while lead [. v.], to which [it] is inferior in covering power, and which [it does] not exceed in permanence . The precise chemical composition seems to be currently unknown. See also lead antimonite. 

Both antimony tribromide and antimony ttiiodide are prepared by reaction of the elements. Their chemistry is similar to that of SbCl in that they readily hydroly2e, form complex haUde ions, and form a wide variety of adducts with ethers, aldehydes, mercaptans, etc. They are soluble in carbon disulfide, acetone, and chloroform. There has been considerable interest in the compounds antimony bromide sulfide [14794-85-5] antimony iodide sulfide [13868-38-1] ISSb, and antimony iodide selenide [15513-79-8] with respect to their soHd-state properties, ferroelectricity, pyroelectricity, photoconduction, and dielectric polarization. 

Amorphous Sb2S2 can be prepared by treating an SbQ solution with 442S or with sodium tliiosulfate, or by heating metallic antimony or antimony trioxide with sulfur. Antimony trisulfide is almost iasoluble ia water but dissolves ia concentrated hydrochloric acid or ia excess caustic. In the absence of air, Sb2S2 dissolves ia alkaline sulfide solutions to form the tliioantimonate(III) ion [43049-98-5], SbS 2, in the presence of air the tetratliioantimonate(V) ion [17638-29-8], SbS , is formed. The lemon-yellow crystalline salt, Na SbS 94420, known as Schhppe s salt [1317-86-8], contains the tetrahedral tetratliioantimonate(V) ion. 

Many metal sulfides when mixed intimately with metal halogenates form heat-, impact- or friction-sensitive explosive mixtures [1], That with antimony trisulfide can be initiated by a spark [2] and with silver sulfide a violent reaction occurs on heating [3], For the preparation of oxygen mixture , antimony trisulfide was used in error instead of manganese dioxide, and dining grinding, the mixture of sulfide and chlorate exploded very violently [4],... 

It may also be prepared by the reaction of antimony pentachloride in HCl with hydrogen sulfide and removing any free sulfur by extraction with carbon disulfide ... 

The pure sulphide is obtained from its ore. Stibnite is separated from other ores by grinding and flotation. The ore is then heated to 550-600°C in a perforated vessel. The pure molten material is collected and cooled. It is also prepared by passing hydrogen sulfide into a solution of antimony trichloride ... 

Potassium chlorate is an oxidizing agent in matches, fireworks and explosives. The head of safety matches is coated with potassium chlorate which is struck on a surface consisting of red phosphorus, antimony(lII) sulfide and an adhesive to light the fire. It also is used in laboratory preparation of oxygen. Its dilute aqueous solution is an antiseptic. 

Triphenyl stibine has been prepared 1 from antimony trichloride and chlorobenzene dissolved in dry benzene in the presence of sodium. This yields triphenyl stibine dichloride, which on decomposition with hydrogen sulfide yields triphenyl stibine. Triphenyl stibine has also been prepared2 by the action of phenyl magnesium bromide and antimony trichloride. 

Three and four-tenths grams of antimony trisulfide is prepared by passing hydrogen sulfide into a solution of 6.6g potassium antimonyl tartrate (4.5g of the trichloride or 2.9g of the trioxide may be used instead) in 2N hydrochloric acid until precipitation is complete. 

The furnace is subjected to a temperature/time treatment according to the specifications given in the tables for the respective compound. For the preparation of antimony(III) iodide sulfide, the furnace is cooled uniformly from 480-250°C. for a period of 10 days. ... 

The compounds have been prepared by annealing stoichiometric amounts of the elements or the respective antimony(III) or bismuth(III) sulfide and halides in sealed silica ampuls.11 12 Good crystals are obtained by using a surplus of M2X3.12 The conditions for the preparation of these thiohalides are given in Table VI. 

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