Aug. 14, 1945. A.

BELcHETz
PRODUCTION OF ANHYDROUS MAGNSIUM CHLORIDE
2,381,9'94
Filed Nov. 21, 1941

ARNQLD BELcHETz
INVENTOR

iBYSM-A
A-rroRNEY
Patented Aug. 14, 1945 2,381,994

UNITED STATES PATENTv OFFICE

PRODUCTION oF A'NnYDRoUs MAGNESIUM

Arnoldelchetz, Kew Gardens, N. Y., assigner `to

This invention relates to the preparation of dehydrating any of the various hydrous form
anhydrous magnesium chloride from hydrous cf magnesium chloride, whereby a product of
forms thereof. The principal object of the in high purity is obtained. The _method of my in
.vention is to provide an economical and com vention involves heating a hydrous form of mag-
mercially practicable method of preparing a pure nesium chloride with'a volatile non-aqueous liq
anhydrous salt, and while not limited thereto, uid in which anhydrous magnesium chloride is
the invention may be employed with particular soluble, to distill off water with vapors of the
advantage in preparing a pure anhydrous mag liquid and leave a non-aqueous solution of mag
nesium chloride for use in the electrolytic manu nesium chloride as the distillation residue. Sep
facture of metallic magnesium. aration of solid anhydrous salt from the non- v
Magnesium chloride is very soluble in water, aqueous solution is thereafter accomplished by
and crystallizes therefrom as' a hexahydrate, vaporizing the solvent. '
MgClaGl-IzO, which is deliquescent. The latter The non-aqueous solvents which I prefer to
substance, containing about 53 per cent water, use in practicing my invention are the saturated
cannot be dehydrated furtherby simple heating monohydroxy aliphatic alcohols, and more spe
without substantially complete decomposition, cically those alcohols of the latter type having
the basic saltl MgzOCh and the hydroxide atmospheric boiling points between 220 and
Mg(OI-I)z being formed with the liberation of hy about 350 F. In the following further descrip
drochloric acid. By spray drying a hot saturated tion of an exemplary embodiment of the inven
magnesium chloride solution, a product contain 20 tion, with reference to the annexed drawing, the
ing about 26 per cent water and corresponding use of such an alcohol will be assumed. As will
approximately t0 a dihydrate (MgClzZHzO) can i' be understood by those familiar with distillation
be obtained. Material produced- in this .way is processes, however, other solvents can be used.
contaminated with about 1 per cent Mg(0l-)a as The annexed drawing is a diagrammatic ilow
e. result of partial hydrolysis. 25 sheet of an exemplary embodiment of the inven
The electrolytic process for the manufacture tion, wherein items of equipment are conven
of metallic magnesium involves passing a cur tionally shown and from which self-evident
rent of electricity through a cell containing a necessaries such as pumps, valves and the like
molten mixture of magnesium chloride,- KCl and have been omitted for greater clarity.
NaCl, the latter two substances being present for 30 The operating step to vbe rst described is es
the purpose of lowering the melting point of the sentially a distillation, and could, if desired, be
magnesium chloride. The cell temperature is carried out as a 'batch operation. For greatest
usually about 1300" F., and it is not feasible to efllciency, however, it is preferable to employ
add magnesium chloride to the cell as hexahy continuous fractionating equipment and to sup
drate, because decomposition t0 the o_xide would 35 ply the feed in the form of a hot aqueous solu
immediately occur. By forming briquettes of the tion of magnesium chloride containing the mini- ~
dihydrated salt prepared as described above, how-Y mum amountof water; that is, to supply
ever, and dropping them directly into the molten MgClzmO
electrolyte at 1300 F., a flash evaporation of the
remaining 26 per cent water is eflected whereby dissolved vin little more than its own water of
only about 2 to 3 per cent more of the magnesium crystallizationL Such a solution may be obtained ,
chloride is decomposed into HCl and MgO. The from a more dilute one by conventional evapora
presence of the later substance .in the cell causes tion methods, or in other ways depending upon
some diiilculty, because it forms a sludge which the original source of the magnesium chloride.
must be drawnoff as it accumulates. The at In the drawing, an aqueous magnesium chlo
tendant formation of hydrochloric acid is much ride solution is takenfrom any available source
more troublesome, however, not only because of and introduced into line l. An alcohol-water
the danger of corrosion, but also for the reason ' mixture derived from a subsequent step of the
that it contaminates the chlorine which is a val process is introduced into line I through line 2,
uable by-product of the `lelectrolysis. As will be and anhydrous alcohol derived from still another
readily understood, therefore, the art has long _ step of the process is introduced into une 'l'
sought a commercially practicable methodof pro through line). The magnesium chloride', water
ducingabsolutely anhydrous magnesium chloride. and alcohol solutionthus formed in line I. is
I have now discovered a relatively inexpensive passed into a sedimen tion drum l wherein any
and eillcient large scale method of completely salts such as sodi chloride, sodium sulfate, -
c
 2 2,381,994
etc., which may have been presentas impurities additional quantities of. magnesium chloride so
' dissolved in the .initial magnesium chloride solu lution, as previously described.
tion are precipitated and settled out by reason ' In order to permit the evaporation of alcohol
of their insolubility in dilute alcohol. Sediment from the magnesium chloride solution in dryer
is periodically drawn off as it may accumulate I2 at the lowest possible temperature, and thus
in the drum`4, by means of line 5, and rejected to inhibit the slight tendency of the salt to react
from the process as waste. If desired, the small _ with certain of the alcohols which may be used,
amount of alcohol accompanying the withdrawn I may, when it is advantageous to do so, main
slurry is recovered by evaporation and returned tain the drying and recovery system under re
to the4 process. It will be seen that my method 10 duced pressure. To this 'end I exhaust vapors
of preparing pure anhydrous magnesium chlo from accumulator 22 by means of compressor 23
ride has the advantage initially of accomplish and by means of line 24 return the compressed
ingthe removal of soluble salts suchas 'are likely vapors to the -base of column 8. Alternatively, I
to be associated with magnesium chloride ob may introduce an inert gas into the ~dryer to
tained by fractional crystallization of brines. In 15 lower the partial pressure of the alcohol vapors
fact, when the source- of magnesium chloride is and carry them oil? more rapidly. In the latter
a mixture of dissolved salts, little or no puri event, of course, compression of the vapors from
fication thereof prior to dehydration may be re the dryer is necessary prior to condensation vof
quired other than that provided bythe above the alcohol therefrom. a'nd the inert gas remain
mentioned precipitation. They sedimentation 20 ing uncondensed is suitably recycled to the dryer.
`drum 4 is alternatively replaced by a iilter if Under certain circumstances, as when the iinal
desired. v anhydrous product is desired in molten rather ~
Magnesium chloride - water - alcohol solution than in pulverulent-~form, I remove only enough
from which insoluble impurities have been re alcohol from the solution supplied to the dryer
moved is passed via line 6 to a preheater 'I where 25 to produce a solid product, which, however, still
in it is heated preferably to its boiling point, -It contains some alcohol. I then nish drying the
is then introduced into the mid-section of a dis solid so obtained, and melt it, by passing it
tillation column 8. The latter can be of con through a conventional heated rotary kiln dryer
ventional design, embodying fractionating bub and discharging it at an elevated temperature.
ble trays, bales, packing or the like. A steam 30 Returning to the distillation column S for a
heated reboiler coil 9 is situated in the base of description of remaining features of'this embodi
column 8 and a water cooled reflux condensing ment of the invention, it will be understood that
coil I0 is located at the top. f the function of the reboiler coil 9 and the vapor
In column 8 the liquid portion of the feed is liquid contact in the lower portion of the column
fractionated into absolute alcohol as the higher 35 is to expel all water'from the feed mixture, so as
boiling bottom product and .a constant-boiling to make possible the withdrawal of an anhydrous
mixture of water and alcohol as the lower-boil alcohol solution as bottom product. As the water
ing top product. The magnesium chloride, being is vaporized and expelled from the feed mixture,
non-volatile, remains in the liquid flowing down there is inevitably a substantial vaporization of
through the column and is withdrawn in an an 40 alcohol also, and _the function o1' the upper sec
hydrous condition, dissolved in absolute alcohol, tion of the column and the redux-condensing
by means of line II. This solution is passed as coil I0 is to prevent, as far as possible, the escape
indicated into an evaporator or dryer I2 of the of alcohol with the water in the overhead vapors.
enclosed, internally heated drum type, and is 45 It so happens that those alcohols which I prefer
therein sprayed onto a drum I3 which is con to employ in practising my invention all form
stantly and slowly rotated by any suitable vmech constant-boiling mixtures with water; that is to
anism acting through a hollow `shaft passing say, in distilling mixtures of these alcohols with
through a stufling box in the side wall of the water, it is not possible to produce both anhy
outer shell of the dryer. Steam 'or other suit drous alcohol and alcohol-free water from `any
able heating medium supplied through line I one alcohol-Water mixture. If the mixture to be
is passed through drum I3 via its hollow carry distilled contains more water (less alcohol) than
ing shaft and it is thereby heated to a tempera the constant-boiling mixture, then it will not Fbe
ture high enough to vaporize the alcohol in the possible to produce anhydrous alcohol as a. prod
solution being sprayed onto it. The construc ufct. The alcohol will be concentrated to the pro
tion of the dryer is exemplary only, and as such portion in which itexists in the constant-boiling
mixture, and the excess water will be produced
devices are well known to the art, extensive ex as a bottom product, free from alcohol if the
planation of their operation is not necessary fractionation is sumciently precise, If on the
herein. . '
other hand the mixture contains less water (more
As alcohol is vaporized and driven oil' from 60 alcohol) thanthe corresponding constant-boiling
Athe liquid sprayed on to the rotating drum I3, mixture, then anhydrous alcohol may bewith
a skin or 'layer of anhydrous magnesium chloride drawn as a bottom product and the constant
is left, and this is removed continuously by a boiling mixture will be the top product, providing
scraper blade I5 riding on the surface of the suiliciently.'v precise fractionation is eiected, In
drum. The dry material thus produced, by a 65 asmuch as the latter situation necessarily must
suitable mechan'ical arrangement such as screw ofbtain in practising my invention, i. e., anhy
" conveyor I6 driven by motor I1, is removed from drous alcohol must be one of the distillation prod
the interior of the dryer and disposed of as de ucts, it is necessary to add to the initial mag
sired via product outlet I8. nesium chloride solution that quantity of alcohol
Alcohol vapors evolved in the drying operation 70 which will be distilled oil with the water to be
pass oil from the drum housing through line 20 removed, in a'constant-boiling mixture. Also, it
and are recovered as a liquid by cooling and con-_ is necessary to add alcohol'in excess of the latter
densation in condenser 2 I. The thus-condensed> quantity, to act as a solvent for the anhydrous
anhydrous' alcohol is collected in accumulator magnesium chloride and prevent it from being
22 and passed via line 3 for r'e-admixture with 75 left as a solid when the water and the iirst quan
 '2,381,994 '.3
tity of alcohol are distilled on'. Unless the column other through the condensation and decantation
is provided with refiuxing facilities, however, the steps.
overhead product will be richer in alcohol than The upper layer of liquid in decanter 23 will
` the corresponding constant-boiling mixture, and at 100 F. consist of a mixture of roughly 90
hence a greater quantity of alcohol would in such per cent alcohol and l0 per cent water, and it is
an event have to be added to the feed. With the this liquid which is passed through line 2 to
higher-boiling alcohols the excess which would be introduced into the feed line l. It will be
be thus necessitated would not be great, and in understood that the anhydrous alcohol recovered
any case the reiiuxing may Ibe omitted if desired. from the dryer and returned through line -3 sup
If no reflux is used the feed may be introduced plies that proportion of alcohol necessary to act
into the top of the column, instead of at a lower as a solvent for the anhydrous magnesium chlo
point. It will be understood that even when re ride, and that alcohol is recovered by decanta
flux is used, the column must contain a sufficient tion in quantity suflicient for the removal of
nuinlber of plates or the like if fractionation of water from the aqueous feed. There are thus
excess alcohol from the top product is to be 15 two closed continuous alcohol cycles. Unavoid
effected able small losses of alcohol from the system are
While I do not wish to be bound by any theory made up by periodic additions, but otherwise
offered herein in explanation of the eiiicacy of the process_'is self-contained asto the water
my invention, it is believed that the mechanism _of removing medium.
water-removal in accordance with the invention The water-removing capacity of the alcohol
is as follows: rich liquid supplied to the feed line from the '
When a hydrous form of magnesium chloride decanter is proportional to the difference be
dissolves in a non-aqueous solvent, the bond of tweenthe percent water in that liquid and the
association between the magnesium chloride and percent water in the constant-boiling mixture.
the water is weakened, and there is a lessened The former ilgure will be, as previously stated,
tendency for the magnesium. chloride to ionize; not far from ten per cent at 100 F. for all the
A hence, water can be expelled from the solution by preferred alcohols. The latter figure ranges
heating and distillation without the occurrence of from about 32 per cent up to 50 per cent and
hydrolysis. It is to be noted that while a volatile higher, whence it will be seen that the alcohol
solvent contributes to the ease with which the wa - 30
saturated with water from the decanter will
ter is removed, by its stripping effect, this in itself in all cases have a water-removing capacity not
is insufficient to account for the avoidance of hy far below that of the absolute alcohol. It is
drolysis, Otherwise, it would be possible to entirely feasible and within the scope of the
achieve equally good results by using reduced
pressure, in place 0f the volatile solvent, to facili invention to produce absolute alcohol from the
upper layer in the decanter by a single extra
tate the vaporization of water at a low tempera
ture; Complete dehydration of magnesium chlo stage of fractionation, the alcohol being ob
ride cannot be accomplished without decomposi tained in such an event as a bottom product,
tion simply by heating it under vacuum. and constant-boiling mixture being obtained as
Referring now again tothe drawing, the top a top-product forcondensationv and return to
of the column is maintained by the cooling effect the decanter. Absolute alcohol so obtained may
of reiiux coil l0 at the boiling point of the con then be introduced into the feed line in lieu of
stant-boiling mixture of alcohol and water which the 90 per cent alcohol employed in the de
constitues the overhead product of the distilla scribed embodiment of the invention. In such a
tion. The column overhead vapors are passed' 45 case a smaller total volume of liquid would have
through line 25 into line 26 and are cooled suit to be introduced and a smaller volume of vapors
ably to about 100 F. and liquefied in a condenser taken overhead. These small economies are not
21, the condensate being then passed through line in` the usual case suiiicient to justify the expense
2B to a settler or decanter 29. Inthe latter vessel, of an additional stage of fractionation, however.
a further property of the preferred alcohols mani (il While I have shown and described an embodi
fests itself. The solubility of these alcohols in ment of my invention wherein the water-remov
water varies ibetween individual members from inging distillation is accomplished with maximum
about 1 per cent to about 4 per centat 100 F. efficiency, it is to be understood that less efll
and the corresponding solubilities of water in the cient arrangement can be operated to obtain a '
4alcohols varies from about 12n per cent to less 55 satisfactory product. For example, it is possible Y
than 10 per cent. Hence, in the decanter 29 there within the scope of the invention to charge solid
will be a separation of the condensate into two MgCl2.6HzO into a shell or pot still lacking
layers, the upper layer being mostly alcohol and any fractionating devices whatsoever, add a sum
the lower layer mostly water. As the water' layer cient quantitylof alcohol, either all at once or
contains less water than the constant-boiling (ll gradually as the subsequent distillation proceeds,
mixture, it is possible as hereinbefore explained and to distill off all thev Water from the hydrate,
to separate it by fractionation into alcohol-free leaving the latter in an alcohol solution. Solu
water as a bottom product and constant-boiling tion of the solid crystalline material initially
mixture as a top product. The lower layer is charged takes place as it is heated with-the al
therefore drawn off through line 30 and rectified cohol to distillation temperature. The quantity
in redistillation column 3l. Reboiler heat is sup of alcohol required to be distilled per pound
plied to column 3l by steam-heated reboiler coil of water removed is much greater in the absence
32, the bottom temperature being substantially ` _ of any fractionation, and therefore the shell still
.the boiling point of water, 212 F. The top of the method is less advantageous. Recovery of the
redistillation column is again maintained at the alcohol by decantation is possible with this
boiling point of the constant-boiling mixture by method, however, just as in the embodiment
means of water cooled reflux condensing coil 33. shown in the drawing. .
VaporrJ from column 3l pass through line 34 to be It is to be understood that the invention is not
combined with vapors from column 8 in line 26, limited tfevaporation as a method of separating
whence they travel in admixture one with the 7.5 anhydrous magnesium chloride- from a non
 4 2,381,994.
aqueous solvent solution, as it is feasible in some desired to be withdrawn. It is preferable to use
cases to add a precipltant, such as carbon di suflicient excess alcohol in the lower alcohol re
_ sulfide, which Iis miscible with alcohol but inca cycle circuit to avoid any possibility of crystal
pable of dissolving magnesium chloride. Also, I lization in line H vor the base of column I. In
may use any-suitable method of evaporation, in asmuch as with iso-amyl alcohol the alcohol layer
cluding spray drying. taken from the decanter will contain l0 per cent
Referring now in somewhat greater detail to water and the distillate vapors will contain 42
the solvents which may be used in practising the per cent water, each pound of alcohol supplied
invention, it will be understood that for maximum to the column from the decanter will be capable
efllciency a solvent should possess a substantial 1,0 of carrying overhead about 0.6 pounds of water
capacity to dissolve magnesium chloride. The in addition to that :which enters with it, assum
normally liquid homologs of methanol are out ing efficient fractionation.
standing in this respect, but the lower-boiling My invention is not limited to any of the em--
members of the group are characterized by low bodiments described herein for illustrative pur
water-removing ability. In the case of methanol,_ 15 poses, but only in and by the following claims,
for example, the tendency of the solvent is to dis wherein I wish to claim all novel features of my
till off in preference to the Water, and the more invention.
I claim: 4
effective the fractionation the less the water con
tent of the distillate vapors. Ethanol is only l. In a method of- preparing anhydrous mag
slightly less subject to this tendency, as it forms 20 nesium chloride from hydrous forms thereof,.the
a constant-boiling mixture containing about 4 improvement which comprises heating a hydrous
per cent water. In order for either of these al form of magnesium chloride with a volatile non
cohols to be- effective, they must _be supplied to aqueous magnesium chloride solvent which is_
the distillation in anhydrous condition and in substantially unreactive with water and distilling
inordinately large quantity. Since both are com off mixed vapors of all the water in said hydrous
pletely miscible with water, neither can'be re magnesium chloride and said solvent V_lille forin
covered in a sui/liciently water-free condition by ing a solution of magnesium chloride'- i'said sol
' simple decantation.
vent.
The propyll and butyl alcohols-,. except for 2. In a method of preparing anhydrous mag
normal and iso-butanol, are only slightly better 30 nesium chloride from hydrous forms thereof the
than methanol and ethanol in water-removing improvement which comprises heating a hydrous
ability, and while some of these are partially form of magnesium chloride with a normally liq
immiscible with water,` none of them -forms an uid monohydroxy saturated aliphatic alcohol and
alcohol layer containing less water than the distilling off mixed vapors of all the water in said
~corresponding constant-boiling mixture. With hydrous magnesium chloride and alcohol while
all the latter alcohols, except for the two noted forming a solution of magnesium chloride in said
above, it is necessary to resort to azeotropic dis alcohol.
tillation or chemical dehydration to recover them 3. A method of preparing anhydrous magne
in sumciently water-free condition for recycling sium chloride from magnesium chloride hexa
to the distillation. Moverover, the propyl and ,40 hydrate which comprises dissolving said hexa
. hydrate in a normally liquid monohydroxy satu
lower alcohols apparently form alcoholates with
magnesium chloride in which the tenacity vof their rated aliphatic alcohol, distilling the thus-pro
attachment to the salt is comparable to that of duced solution to drive off water therefrom and
Water itself. Hence, their removal by evapora-_ leave a liquid distillation residue consisting of
tion is extremely dimcult. anhydrous magnesium chloride dissolved in alco
I particularly prefer the amyl alcohols or hol, and separating anhydrous magnesium chlo
pentanols as solvents. Hexyl alcohols can be ride from said liquid residue.
used but because of their generally higher cost 4. A method of preparing anhydrous magne
are not conducive to an economical operation. sium chloride from an aqueous solution thereof
Exemplary operating conditions will now be given which comprises mixing said solution with a nor
for the use of iso-amyl alcohol in the previously mally liquid monohydroxy saturated aliphatic al
shown and described embodiment of the inven cohol and distilling off all water from the mixture
tion. The significant properties of iso-amyl alco together with a portion of the alcohol and there
by forming an anhydrous solution of magnesium
hol are as follows: chloride in alcohol, and then evaporating said an
1. Its boiling point is 267 F. hydrous solution to recover anhydrous magne
2. It forms a constant boiling mixture with water sium chloride free from alcohol.
consisting of about 58 per cent alcohol and 5. A method of preparing anhydrous magne
about 42 per cent water, and having a boil sium chloride from an aqueous magnesium chlo
ing point of 203 F. 60 ride solution which comprises introducing said
3. It dissolves water to the extent of about l0 per solution into a distillation zone, introducing a nor
cent by weight at 100 F. mally liquid monohydroxy saturated aliphatic
4. It is soluble in water to extent of about 2 per alcohol into said zone, supplying heat to said
cent by weight at 100 F. zone to vaporize and distill water and alcohol
5. It will dissolve upwards of 16 per cent by therefrom, withdrawing an anhydrous solution
weight of magnesium chloride at itsboiling of magnesium chloride in alcohol from said zone,
point. ' _ separating alcohol from the anhydrous magne
Referring now again to the drawing, with iso sium- chloride in the withdrawn solution and re
amyl alcohol as the solvent the top temperatures turning the separated alcohol to the distillation
of columns B'a'nd 3| should be maintained at 70 zone, condensing the >vapors distilled from said
203 F. The bottom temperature of column 8 zone and returning the alcoholic content ofthe
will, because of the boilinglpoint raising eiect of condensate to the distillation zone.
the dissolved magnesium chloride on the alcohol, 6. A method of preparing anhydrous magne
be higher than 267 F. in any case and> will de sium chloride which comprises heating a hydrous l
pend upon how nearly saturated a solution is 76 form of magnesium chloride with a normally liq
 2,381,994 ,5
uid monohydroxy -saturated aliphatic alcohol 15. A method as in claim l0 wherein said *alco
boiling above 220 F. and distilling ci! all the hol is an amyl alcohol.
water in said hydrous .material in admixture ' 16. A method of v`removing impurities fromA
with vapors of said alcohol, thereby forming an magnesium chloride which comprises forming
anhydrous solution of magnesium' chloride in an aqueous solution of impure magnesium -chlo
said _ alcohol, and then separating anhydrous ride and adding a normally liquid monohydroxy
magnesium chloride from said alcohol. ' saturated aliphatic alcoh'ol to said solution to
. '7. In a method of preparing anhydrous mag precipitate alcohol-insoluble impurities there
nesium chloride from hydrous forms thereof, the
. improvement which comprises heating a hydrous 1'7. A method of preparing anhydrous mag
form of magnesium chloride with a normally nesium chloride which comprises forming a rela
liquid monohydroxy saturated aliphatic alcohol tively concentrated aqueous solution of mag- -
boiling above 220 F. and distilling oi mixed nesium chloride, adding to said aqueous solution>
vapors of water and alcohol while .forming a a quantity of saturated monohydroxy aliphatic
solution of magnesium chloridein said alcohol. , alcohol boiling between220? and 350? F. to form
8. A method of preparing anhydrous mag an aqueous alcoholic magnesiumv chloride solu--
nesium chloride from magnesium chloride hexa tion wherein theproportion of alcohol to water
hydrate which comprises dissolving said hexa is substantially greater than in a constantboil
hydrate in a normally liquid monohydroxy sat ing mixture of said alcohol and water, frac
urated aliphatic alcohol Aboiling above 220 F., tionalling distilling said aqueous'alcoholic solu
distilling the thus-produced solution to drive oil tion to produce an anhydrous solution of mag
water therefrom and leave a liquid distillation nesium chloride in alcohol'as the higher-boiling
residue consisting of a solution oi' anhydrous product and a mixture -of alcohol and water as
magnesium chloride in alcohol, and separating the lower-boiling product, allowing said lower
anhydrous magnesium chloride from said liquid 25 boiling product to separate into a lighter alcohol
residue. A ' ' rich phase and a heavier phase of low alcoholic .
9. A method of preparing anhydrous mag ' content, evaporating and recovering alcohol
nesium chloride from an aqueous solution there -from said anhydrous solution to leave anhydrous
of which comprises mixing said solution' with a v ` magnesium chloride free from alcohol, and using
normally liquid monohydroxy saturated >aliphatic the thus-recovered alcohol and alcohol-rich
alcohol boiling above 220 F. and distillir'igr oi phase to form additional amounts of aqueous
all the water from themixture together with a ' alcoholic magnesium chloride for treatment as
portion of the alcohol, thereby> forming an an aforesaid. y
hydrous solution of magnesium chloride in alco 18. A method of preparinganhydrous mag
hol, and then evaporating said anhydrous solu nesium chloride yfrom a hydrous form thereof
tion to recover the anhydrous magnesium chlo containing alcohol insoluble impurities which
ride free iromalcohol. ' comprises mixing said impure hydrous mag
10. A method of preparing anhydrous mag nesium chloride with a normally liquid mono
' nesium chloride. from an aqueous magnesium hydro'xy saturated aliphatic alcohol boiling above
chloride solution which comprises introducing 40 220 F'._to precipitate the alrohol insoluble im
said solution into adistillation zone,- introducing purities therefrom, removing said precipitated
a normally liquidv Vmonohydroxy saturated _ali impurities, introducing the thus purified hydrous
phatic-alcohol boilingabove 220 F. into said magnesium chloride together with the admixed
zone,_supp1yins heat to said zone to vaporize and alcohol into a distillation zone, supplying heat '
' distill vWater'and alcohol therefrom, withdrawing 45 to said zone to vaporize andl distill off all of the4
anv anhydrous solution of magnesium chloride. water in said hydrous magnesium chloride in
in lalcohol from said zone, separating alcohol admixture with vapors of said- alcohol, withdraw
from said anhydrous solution, and returning the,l ing a solution of anhydrous magnesium chloride
' separated alcohol'to the distillation zone, con in anhydrous alcohol from said zone and thenl y
densing the vapors distilled from said zone and 50 recovering the anhydrous magnesium chloride
allowing the condensate to separate into an alco from said. withdrawn solution.
hol-rich phase and an aqueous phase, and re 19. A method of preparing anhydrous mag
turning- said alcohol-rich phase to said distilla nesium chloride which comprises heating a hy
tion zone. ' . Y drous form of magnesium chloride with a nor
11.v A method as in claim 6 wherein said alco-l mally liquid monohydroxy saturated aliphatic-v
hol is an amyl alcohol. alcohol andv distilling oil.' all the water in said 'i
12. A method asin claim 7 `wherein said alco hydrous material in admixture with vapors of
vhol is an amyl alcohol. said alcohol, 'thereby forming> an anhydrous
13. A method as in claim 8 wherein said alco solution of magnesium chloride in said alcohol,
hol is an amyl alcohol. . . \ so and then recovering magnesium chloride from
14. A method as in claim 9 wherein said alco , said solution.
hol is an amyl alcohol. ARNOLD am. '