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[OCTACHLOROHEXAMOLYBDENUM(II)CHLORIDE]
Mo 52 Cl 2 MoCl5
3 MoCl5 2 Mo 5 MoCl3
6 MoCl3 3 MoCl5 (Mo 6 Cl 8 )Cl 4
Reagent required :
1. 8 g 0f powdwred molybdenum metal
2. Chlorine cylinder
3. Nitrigen cylinder
Special apparatus required :
1. Tube furnace
2. Vycor or silica tube
3. Thermocouple and pyrometer
4. Porcelain boat
5. Vacum pump with cold trap
6. Abderhalden drier
PROCEDURE
The apparatus show in fig. 1 is assembled. The molybdenum powderis placed in
the boat, and the boat is placed in the middle of vycor tube, centered in the tube furnace.
The rubber stppers at each end of the vycor tube are coated on the inside with paraffin
wax or kel-F grease.
A stream of chlorine gas is passed through the tube at the rate ofabout four
bubbles per second. After several minutes, the tube furnace is turned on. And the
temperature is adjusted to about 500o with the aid of a powermite or variac. Soon dark
green and red-brown crystals will deposit in section B of the tube. After about 20 min or
when the tube is opaque with crystals to within about 5 cm of the stopper on side B, the
flow of chlorine is stopped and the tygon tubing from the bubbler is disconnected from
the glass tubing attached to side A. Immediately, the delivery tube from the nitrogen
bubbler is a attached to side B, and a stream of nitrogen (about four bubbles per second)
is passed through the tube in a direction opposite to the original chlorine flow. When all
the chlorine has been flushed from the tube, the furnce temperature is increased to 600700o andside B is heatedwith the hot flame of a fisher burner to drive the MoCl 5 through
the furnace to side A. A residue of MoCl 3 (brown red) and (Mo6Cl8)Cl4 (yellow) in side B
will probably remain. The nitrogen delivery tube is then switched to sideA and the
flaming procedure is repeated on side A. to drive the MoCl 5back to side B. The MoCl5 is
repeatedly passed over the hot molybdenum in this way until most of it has been reduced
to the less volatile MoCl3 Care must be taken not to allow the rubber stoppers to become
not. Finally with nitrogen entering side A, side A heated very strongly with burner until
practically all the material turns yellow. Then with the nitrogen flowing in the same
direction. Side B is similarly heated, allowing the unreacted MoCl 5 to escape out the exit
tube of side B.
The tube is cooled to room temperature; the stoppers a removed from the ends of
the tube, and the boat containing the residual molybdenum is pulled out of the tube with
a long wire with a hook at the end. Then a solid rubber stoppers is attached to one end of
the tub, and about 100 ml ofwarm (50o) 6 M HCl is poured into the tube. The other end
of the tube is stoppered and the aqueous acid is sloshed around the tube dissolve the
yellow (Mo6Cl8)Cl4. If all the (Mo6Cl8)Cl4 does not dissolve more aqueous HCl is added.
The solution is filtered, evaporated on a hot plate to one-fourth the original volume of
the solution and the cooled in a ice bath. The precipitate f bright yellow (H 3O)2
diputuskan dari tabung gelas yang terpasang ke sisi A. Dengan segera tabung pengiriman
dari pembuat gelembung nitrogen dipasang ke sisi B dan arus Nitrogen (sekitar4
gelembung /detik) dilewatkan melalui tabung dalam arah berlawanan dengan aliran
Klorin. Ketika semua Klorin telah bersih dari tabung vycor, suhu tabung meningkat
menjadi 600-700o dan sisi B dipanaskan dengan api panas dari sebuah pembakar fisher
untuk menggerakkan MoCl5 melewati tanur disisi A. Residu MoCl 3 (merah-kecoklatan)
dan (Mo6Cl8)Cl4 (kuning) disisi B kemungkinan akan tersisa. Tabung pengirim nitrogen
kemudian dialihkan kesisi Sdan Prosedur pembakaran diulangi disisi A untuk
menggerakkkan MoCl5 kembali kesisi B. MoCl5 berulang kali dilewatkan melalui
molebdenum panas sampai semuanya direduksi menjadi MoCl3 yang sulit menguap.
Sumbat karet tidak boleh sampai panas. Akhirnya, dengan masuknya nitrogen ke sisi A
dan sisi A dipanaskan dengan sangat kuat dengan menggunakan pembakar sampai
material berubah menjadi kuning. Kemudian dengan mengalirnya nitrogen dalam arah
yang sama,sisi B juga ikut terpanasi, memungkinkan MoCl5 yang tidak bereaksi keluar
dari tabung disisi B.
Tabung didinginkan sampai mencapai suhu kamar, sumbat karet dilepas dari
ujung-ujung tabung dan biduk yang berisi sisa-sisa Mo didorong keluar tabung dengan
kabel panjang dengan pengait diujungnya. Kemudian salah satu sumbat karet dipasang
pada salah satu ujung tabung dan sekitar 100 ml HCl 6 M hangat (50 o)dituang kedalam
tabung. Ujung tabung yang lain disumbat dan larutan asam dikocok dalam tabung untuk
melarutkan (Mo6Cl8)Cl4 kuning. Jika semua (Mo6Cl8)Cl4 tidak larut, ditambahkan lebih
banyak larutan HCl. Larutan tersebut disaring, diuapkan pada wadah panas sampai
dari volume awal larutan. Kemudian didinginkan dalam pendingin. Endapan dari (H3O)2
ini.
Senyawa
seperti
[(Mo6Cl8)(OH)4(H2O)2].
12
H2O,