GrayGhost-
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Ethylbenzene
Hi people
I find a datasheet of commercial product, is solvent por epoxy, composition variable in percentage:
xylene 50 -70%
2 etoxyetanol 20-30%
ethylbenzene 10-20%
ethanol 1-5 %
butanone 1-5%
My question : If posible obtain via simple or fractionated distillation ethylbenzene?
Thanks.
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JJay
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It is pretty hard to separate it from xylenes. You might find a way to do it with azeotropes and fractional distillation.
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GrayGhost-
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Quote: Originally posted by JJay  | | It is pretty hard to separate it from xylenes. You might find a way to do it with azeotropes and fractional distillation. |
Xilene bp 144°C, Ethylbenzene pb 136°C only 8 °C.  this is razon.
Thanks JJay.
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Corrosive Joeseph
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"As is seen in Table A - l , ethylenic double bonds were easily hydrogenated in high yields; for example, ethylbenzene was obtained in an 81.4% yield
from styrene.
Experimental - The Reduction of Styrene.
A suspension of styrene (10 g) in 100 ml of water was refluxed vigorously in the presence of ppt-Ni containing 4 g of nickel. After the solution had
been refluxed for 12 hours, the ppt-Ni was separated by filtration while hot, and washed with water and then with ether. The filtrate and the washings
were combined and extracted with ether. The extract was dried over anhydrous magnesium sulfate, and the ether was carefully evaporated away on a water
bath. The residue was analyzed by gas chromatography."
Taken from - "New Hydrogenating Catalysts (Urushibara Catalysts) - Kazuo Hata 1971"
https://www.sciencemadness.org/whisper/viewthread.php?tid=84...
/CJ
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GrayGhost-
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| Quote: Originally posted by Corrosive Joeseph | "As is seen in Table A - l , ethylenic double bonds were easily hydrogenated in high yields; for example, ethylbenzene was obtained in an 81.4% yield
from styrene.
Experimental - The Reduction of Styrene.
A suspension of styrene (10 g) in 100 ml of water was refluxed vigorously in the presence of ppt-Ni containing 4 g of nickel. After the solution had
been refluxed for 12 hours, the ppt-Ni was separated by filtration while hot, and washed with water and then with ether. The filtrate and the washings
were combined and extracted with ether. The extract was dried over anhydrous magnesium sulfate, and the ether was carefully evaporated away on a water
bath. The residue was analyzed by gas chromatography."
Taken from - "New Hydrogenating Catalysts (Urushibara Catalysts) - Kazuo Hata 1971"
https://www.sciencemadness.org/whisper/viewthread.php?tid=84...
/CJ |
Very interesting procedure  , thanks Corrosive J. the more complicated is
preparation of Urushibara nickel.
[Edited on 3-8-2018 by GrayGhost-]
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JJay
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Some xylenes boil at lower temperatures. You could probably fractionally distill ethylbenzene from o-xylene, but m- and p-xylene boil at 139 C and 138
C, respectively. That's a tough distillation.
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GrayGhost-
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| Quote: Originally posted by JJay | | Some xylenes boil at lower temperatures. You could probably fractionally distill ethylbenzene from o-xylene, but m- and p-xylene boil at 139 C and 138
C, respectively. That's a tough distillation. |
I dont know what type o mixture of xilene is that product, is expensive, possibly I tempt hydrogenate styrene more ahead. I read what Urushibara
Cobalt and Iron can work. Iron salt are more cheaps.
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Corrosive Joeseph
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"10 grams of Zinc dust, as fine as possible, and about 3ccs of distilled water are put in a 100cc RBF and heated on a boiling waterbath.
A stirrer reaching the bottom is installed.
10cc of an aqueous solution containing 4.04 grams of Nickel Chloride, NiCl2-6H20, is heated to ebullition (boiling or bubbling), and added to the Zinc
dust by means of a pippette, with vigourous agitation in a few sec.
The solids are at once collected on a glass filter by suction, washed with a small quantity of hot distilled water, transferred into 160cc of 10%
aqueous caustic soda contained in an erlenmeyer flask as quickly as possible, and digested at 50-60 degreesC for 15-20 minutes with ocaissional
stirring.
Then, the supernaturant liquid is removed, and the solids are washed with 40cc of distilled water of 50-60 degreesC two times, and finally with the
solvent of hydrogenation, eg. ethanol. The rinsings are always removed by decantation.
In this way, a catalyst consisting of about 1 gram of Nickel and 4.7 grams of Zinc, and acting as good as 1 gram of Raney Nickel catalyst (eg. W-7),
is obtained and can be used for hydrogenation or reduction of ketones, nitriles, oximes and double bond conjugated with carbonyl or carboxyl group at
ordinary temperature and pressure"
Taken from - "Procedure for the Preparation of the New Nickel Catalyst" - Urushibara and Nishimura (1954)
"As for the soluble nickel salt, the chloride, nitrate, sulfate, and acetate were successively employed, and nickel chloride was found to be the most
appropriate for obtaining a catalyst of high activity. Nickel nitrate solution hardly reacts with zinc dust, and nickel sulfate solution yields a
catalyst of rather low activity. Nickel acetate, on the contrary, readily yields precipitated nickel, which proves to give as good a catalyst as that
obtainable from nickel chloride."
Taken from - 'Preparing Urushibara catalyst' thread @ The Hive
/CJ
[Edited on 4-8-2018 by Corrosive Joeseph]
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unionised
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You can probably freeze most of the p xylene out of a mixture, but separation of m xylene from ethylbenzene is going to be a real struggle.
What do you want ethylbenzene for?
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GrayGhost-
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| Quote: Originally posted by unionised | You can probably freeze most of the p xylene out of a mixture, but separation of m xylene from ethylbenzene is going to be a real struggle.
What do you want ethylbenzene for? |
Every synth of mine is like a trophy.
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