Patented Apr.

5, 1932 1,852,183

UNTED STATES PATENT OFFICE

GEORGE E. MILLER AND SAMUEL C. WITHERSPOON, OF EDGEWOOD, MARYLAND
2.

PROCESS FOR PREPARING ARSENIC TRICHLoRIDE

No Drawing. Application filed September 25, 1928. Serial No. 308,334.
(GRANTED UNDER THE ACT OF MARCH 3, 1883, ASAMENDED APRIL 30, 192S; 3700. G.75?)
This invention described herein may be the invention within the scope of the append
manufactured and used by or for the Govern led claims.
ment for Government purposes, without The process forming the subject matter of
payment to us of any royalty thereon. this invention consists essentially in the prep
This invention relates in general to a meth aration of arsenic tri-chloride, by the chlorin-5,5 5
od of preparing arsenic compounds, and more ation of arsenic tri-oxide to form arsenic tri
particularly has reference to a process for chloride, using sulpl ur as a dioxidizing agent
forming arsenic tri-chloride. and arsenic tri-chloride as a solvent.
Previous to this time, arsenic tri-chloride in preparing arsenic tri-chloride accord
has been prepared by treating arsenic tri-OX ing to this invention, Sulphur and arsenic tri to
ide with hydrochloric acid, a process in which oxide are combined either in suspension in a
a dehydration operation is essential, and also liquid Oi in a. solution so that intimate con
by heating arsenic tri-oxide with sulphur tact with chlorine may be obtained. It is
mono-chloride, in which it is necessary to pre preferred that the sulphur and arsenic tri
pare the sulphur chloride in a separate step. Oxide be put in Solution in arsenic tri-chlo
When this reaction reaches completion the ride. If a sufficient quantity of arsenic tri
major portion of the sulphur, added as sul chloride to dissolve the arsenic tri-oxide and
phur chloride, remains in the reactor as free sulphur is employed, and the solution is heat
sulphur. This reaction takes place in ac ed to the boiling point of the arsenic tri
2 cordance with the following equation: chloride and chlorine is passed into the mix, O
6S.Cl -- 2A S.O.-->4 AsCl, -- 3SO, -- 9S the formation of arsenic tri-chloride
place. -
takes
. ...
In the above outlined process the sulphur When chlorine is passed into the solution
chloride is first prepared in a separate op or suspension of arsenic tri-oxide and sul
eration as previously described, and the free phur in arsenic tri-chloride, and the solution. 73
sulphur left from the reaction must be chlo is heated to the boiling point of the arsenic.
rinated for further use as sulphur chloride. tri-chloride, the chlorine reacts with the sul
An object of this invention is to provide phur to form sulphur chloride, which in turn
a method of preparing arsenic tri-chloride. reacts with the arsenic tri-oxide to form ar-,
Sti Another object of this invention is to pro senic tri-chloride. By properly regulatings8.
vide a method of preparing arsenic tri-chlo the proportion of the Feactants, no residue is
ride in which the reaction proceeds quanti left after the distilling of the arsenic tri
tatively. chloride. The reaction forming the subject
A further object of this invention is to matter of this invention may be expressed by
provide a process of preparing arsenic tri the following equation:
chloride in which the anhydrous compound is
formed in a single operation. -
With these and other objects in view which In carrying out this process it is preferred
may be incident to these improvements, the to use the following proportions of arsenic.
invention consists in the method of prepar tri-oxide, sulphur, and arsenic tri-chloride:
ing arsenic tri-chloride to be hereinafter set 606 parts by weight arsenic tri-oxide,
forth and claimed, with an understanding 134 parts by weight sulphur, .
that the several necessary steps comprising 772 parts by weight arsenic tri-chloride.
the invention may be accomplished in any The yields of arsenic tri-chloride which
other order found most suitable for carrying may be obtained by this method equal ap 95
the same into practical effect, and it is appar proximately the theoretical maximum and the
ent that the certain compound and elements product obtained is completely anhydrous
may be substituted for those enumerated and and contains but an unappreciable amount of
ov
Sulphur. In this process free chlorine, sul 00
similar formations effected without limiting phur and arsenic tri-oxide are made to com
 2 1,852,188
bine in one operation with the production of
arsenic tri-chloride, obviating the necessity
of rechlorinating residual sulphur produced
by the old reaction.
s There is accomplished by this invention a
process of making arsenic tri-chloride in a
single operation by the chlorination of arsenic
tri-oxide with chlorine, using sulphur as a
deoxidizing agent and arsenic tri-chloride as
10 a solvent in which no appreciable quantity
of residual sulphur remains, and the product
is obtained directly in an anhydrous condi
tion. .
While we have shown and described the
Is preferred embodiment of our invention, we
wish it to be understood that we do not con
fine ourselves to the precise details of the
process herein set forth, by way of under
standing, as it is apparent that many changes
20 and variations may be made therein, by those
skilled in the art, without departing from
the spirit of the invention, or exceeding the
Scope of the appended claims.
We claim as our invention:
25 1. A method of preparing arsenic tri
chloride comprising combining arsenic tri
oxide and sulphur in solution with arsenic
tri-chloride, heating the solution to the boil
ing point of the arsenic tri-chloride and
30 chlorinating the mix. is
2. A method of preparing arsenic trichlo
ride comprising combining arsenic trioxide
and sulphur in solution with arsenic trichlo
ride, heating to the boiling point of arsenic
35 trichloride passing chlorine into the solu
, tion and distilling off arsenic trichloride.
In testimony whereof we affix our signa
tures.
GEORGE E. MILLER.
40 SAMUEL C. WITHERSPOON.

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