ChemicalBook CAS DataBase List Dimethyl trisulfide

Dimethyl trisulfide synthesis

14synthesis methods

Product Name:Dimethyl trisulfide
CAS Number:3658-80-8
Molecular formula:C2H6S3
Molecular Weight:126.26

It is produced by the microorganism, L. cremoris S2.

67-56-1 Synthesis

67-56-1
792 suppliers
$9.00/25ml

74-93-1 Synthesis

74-93-1
149 suppliers
$454.02/5MG

75-15-0
273 suppliers
$40.00/100g

624-92-0 Synthesis

624-92-0
348 suppliers
$26.39/5ml

3658-80-8
274 suppliers
$34.00/5g

Yield:624-92-0 94.9%

Reaction Conditions:

Stage #1: methanol;methylthiolwith hydrogen sulfide;aluminum oxide with 14percent by weight of potassium tungstate at 400;
Stage #2: with sulfur;N-cyclohexyl-cyclohexanamine

Steps:

1 1. Example in a Continuous Experimental Plant

The two-stage dimethyl disulfide (DMDS) synthesis was carried out in a continuously operating laboratory apparatus which comprises all components of the flow diagram (FIG. 1). [00054] The MeSH tubular reactor (600 mm long, 25 mm in diameter) was filled with a self-prepared catalyst of aluminum oxide with 14% by weight of potassium tungstate. At a temperature of 400° C. (middle of the reactor) and a pressure of 1.1 bar_abs48 g/h (1.5 mol) of gaseous methanol, 34 g/h (1 mol) of hydrogen sulfide and 40 g/h of back gas from the reaction column (composition: 72% of H₂S, 12% of MeSH, 16% of dimethyl sulfide (DMS), small amounts of methanol and dimethyl ether) were fed into the tubular reactor. The gas composition at the reactor outlet was: 13.0% of H₂S, 50.8% of MeSH, 10.3% of DMS, 21.6% of H₂O, 2.4% of MeOH, 1.2% of dimethyl ether (DME). [00055] This gas enters the lower section of the reaction column (bubble-cap column containing 20 plates) and flows countercurrently to the downwardly flowing sulfur solution (still solution from distillation column, to which 19 g/h of sulfur and 0.1 g/h of dicyclohexylamine is metered in), where MeSH reacts with formation of H₂S. The gas exiting at the top of the column and having the composition above is compressed, as back gas, and returned to the MeSH tubular reactor, where a relatively small proportion of the gas is removed from the system. The still solution heated to about 90° C. is two-phase, the upper phase being the water formed in the MeSH synthesis. The phases are passed to a phase separator, where they are separated and the upper, aqueous phase is collected in a discharge container (26 g/h). The lower organosulfur phase is passed at the side to a distillation column which is operated at subatmospheric pressure (300 mbar). The product DMDS was isolated in a sidestream takeoff (53 g/h) and had a purity of 99.6% (0.1% of dimethyl trisulfide, 0.3% of low-boiling components such as dimethyl sulfide (DMS), MeSH, CS₂). The yield of DMDS, based on the sulfur used, is thus 94.9%. The low-boiling components produced at the top of the distillation column were in this case not recycled to the top of the reaction column as in FIG. 1.

References:

US6686506,2004,B1 Location in patent:Page column 5

74-93-1 Synthesis

74-93-1
149 suppliers
$454.02/5MG

624-92-0 Synthesis

624-92-0
348 suppliers
$26.39/5ml

3658-80-8
274 suppliers
$34.00/5g