April 22, 1947. A.

BELCHETZ 2,419,310
SULPHUR PRODUCTION
4. Sheets-Sheet l

z12?
INVENTOR

BY
.7/????
ATTORNEY.
April 22, 1947. A, BELCHETZ 2,419,310
SULPHUR PRODUCTION

Filed Nov. 7, 1944 4. Sheets-Sheet 2

INVENTOR.
Arno?af Age/c/e72
BY
??? ?? ?
477 OAKAVAE)1
April 22, 1947. A, BELCHETZ 2,419,310
SULPHUR PRODUCTION
Filed Nov. 7, 1944 4. Sheets-Sheet 3

?z ,

INVENTOR.

BY
//
April 22, 1947. A, BELCHETZ 2,419,310
SULPHUR PRODUCTION

62

92
Patented Apr. 22, 1947 2,419,310

UNITED STATES PATENT OFFICE 2,419,310

SULPHUR PRODUCTION
Arnold Belchetz, Larchmont, N. Y., assignor to
Stauffer Chemical Company, a corporation of
California,
Application November 7, 1944, Serial No. 562,375
24 Claims. (Cl. 23—224)
2
This is a continuation in part of my applica erable, for the process of this invention enables
tion Serial No. 518,081, filed January 13, 1944. a sulphur to be produced which initially has such
This invention relates to the production of Sul a high insoluble sulphur content that the prod
phur and to improvements in the methods of uct can be used directly, and one does not have
producing that form of sulphur which is identi to resort to an expensive concentration operation.
fied as insoluble sulphur by its insolubility in car However, if desired, the concentrating operation
bon disulphide. Frequently, this material is re can be practiced as part of the process of this in
ferred to as sulphur mu. The invention is also -Vention, thus materially simplifying the equip
concerned with production of a finely divided ment and the process required.
form of sulphur suitable for utilization in place 0. It is the general and broad object of the pres
of flowers of sulphur and other fine sulphurs pro ent invention to provide a novel process for the
duced by chemical precipitation or by mechanical production of finely divided sulphur.
methods such as milling, and grinding. A further object of the present invention is
I have found that by quenching Sulphur vapor to provide an improved process for production of
in a suitable non-aqueous medium such as carbon 5 insoluble sulphur.
disulphide, the proportion of insoluble sulphur The invention includes other objects and fea
produced can be considerably increased over that tures of advantage, Some of which, together with
secured, for example, upon quenching Sulphur Wa the foregoing, will appear hereinafter wherein. I
por in ice water. The operation is Carried on by have outlined the preferred manner of practicing
ejecting a high velocity stream of sulphur in gase 20 the invention.
ous form onto or into a non-reactive liquid which In the drawings accompanying and forming a
is vaporized at least in part, advantage being . palit hereof, and in which the same numerals indi
cate like parts or units, Figures 1, 2, 3 and 4
desirably taken of the latent heat of vaporization
of the quenching medium to cool the Sulphur. are diagrammatic apparatus representations ill
This enables the sulphur to be rapidly lowered in 25 lustrating various apparatus and flow sheets
temperature below the melting point of sulphur which can be employed.
and below the temperature at Which rapid rever THE QUENCHING OPERATION
sion of the insoluble form to the Soluble form of Referring particularly to Figure 1; I have shown
sulphur occurs. The product is, therefore, gener
ally characterized by a very highlinsoluble sulphur 30 a tank 6 having a conical bottom. Extending ver
content, although the process can be so operated tically and depending for a short distance into
as to produce soluble sulphur in large amounts. tank 6 is a vertical tower 7, generally much
The product secured is of a size suitable for use Smaller in diameter than the tank 6 and includ
in place of flowers of sulphur orother fine sul ing a baffled section indicated at 8. A vaporized
35 Sulphur inlet 4 is provided in the bottom portion
phurs. ^ ?, ?

The process of this invention has inherently Of ???! 7, Sulphur being supplied from a vapor
numerous advantages. For example, flowers of izer I 0.
sulphur are commonly produced by cooling sul Inasmuch as the nature of the apparatus will
phur vapor in large brick chambers. This is a be made clearer, I will proceed with a further de
batch operation and is consequently relatively ex 40 scription of the process and operation of the ap
paratus: . .
pensive; also, the capital investment required for
practice of this batch process is considerable. In To start the apparatus into operation, the sev
addition, the product of this invention is useful eral unitS mentioned are first purged with an
in the place of those forms of sulphur now. pro inert gas such as carbon dioxide or an oxygen
duced by chemical precipitation or by grinding 45 free, cold combustion gas; tank 6, is then filled
and milling solidified masses; these operations With carbon disulphide or other suitable liquid,
are likewise costly, requiring either involved chem up to about the level indicated by line 6. Water
ical reaction apparatus or utilization of heavy, is then placed upon the top of the carbon di
expensive mills operated only with considerable Sulphide in the open portion of tank 6; this forces
power input, and requiring the presence of an 50 carbon disulphide up into the tower 7. Upon in
inert atmosphere in the grinding-separating sys troduction of sulphur vapor through inlet f4, the
tem. Further, the advantage of the present in temperature of the carbon disulphide body rises
vention in enabling the quantity of insoluble sul and carbon disulphide is vaporized and passes
phur to be increased over that produced by upWardly through the tower 7 to issue through
quenching sulphur vapors in ice Water is consid 55 line 2 and pass into the carbon disulphide con
 2,419,310
3 4.
denser indicated at: 22. The liquidi fraction con SEPARATION Oz SOLUBLE AND INSOLUBLE FRACTIONS
densed is collected in tank 25 and returned It is also possible to treat the removed slurry to
through line 23 into the top of the tower through produce Separate Soluble and insoluble Sulphur
Sprayheads 24A and 26B. The carbon disulphide fractions. To accomplish this, for example, that
So introduced into the tower acts as a scrubbing portion of carbon disulphide removed through
liquid to Wash down any Sulphur particles rising line 28 is introduced into the upper portion of
through the scrubbing tower as well as to main a washer 29 wherein it is washed with fresh, sul
tain the proper content of carbon disulphide in phur-free carbon disulphide introduced through
the tank S. line 3 i frori line 23 to dissolve the Souble Sul
A precipitate of insoluble Sulphur is formed in phur. The insolubie Sulphur is removed as a
the carbon disulphide and the soluble Sulphur Slurry in clean carbon disulphide from the bot
content of the carbon disulphide gradually in tom of the washer through line 33, while the
creases. If the carbon disulphide is not circulated Sulphur Saturated carbon disulphide is removed at
to a Sufficient rate it will be come Saturated with the top of the Washer through line 3, into a
soluble Sulphur and both the soluble and in 15 water-sealed vessel 36. From the bottom of the
soluble forms of Sulphur will precipitate to form vessel 3 the Solution is taken off by pump 37, a
a slurry in the tank. An agitator 39 maintains portion being returned through line 38 to pro
the slurry in Suspension until it is removed by vide a recycle to the Scrubbing tower i while an
pump 2 which forces the surry out through line other portion is introduced through line 46 into
28 into a washer 29. It is necessary to maintain 20 a fractionating tower . The fractionating
the quantity Cfundissolved Sulphur in the carbon tower includes a reboiler section 42 including a
disulphide slurry Within suitable limits So that Suitabie steam heating coil. Soluble Stilphur col
it can be pumped. About 3.5 pounds of undis lects in the bottom of the tower and is returned
Solved or SUSpended Sulphur per gallon of carbon in molten foim through line 3 to the Sulphur
disulphide solution is the limit of fluidity. I pre wagorizer or to the Sulphur melter 44 where
fer to keep the suspended sulphur content be it mixes with the crude sulphur introduced by
twee?í 1 and 2.5 pounds per gallon of carbon di conveyor 46 to provide a feed for the sulphur
sulphide; the extreme limits are between 0.01. vaporizer. Carbon disulphide vapors released
pound and 3.5 pounds when carbon disulphide is from the fractionating tower paSS through line
employed as the quenching nedium. 5 into line 2 and are condensed with the other
EFFECT of RETENTION Vapors in that line in the conden ser 22. A por
tion of the material forced through line 23 is re
The product initially formed in tank 6 is a turned through line 5 as reflux to the tower 4.
finely divided focculent material somewhat rub The slurry removed through line 33 by pump
bery and plastic. I have found that by retaining 53 is sprayed through distributor jets 54 onto a
it at an elevated temperature for a sufficient rotating drun drier S. To maintain a high cir
period it loses its rubbery characteristic and be culation rate through the distributor 54 a return
comes a well dispersed finely divided non-plastic line 53A is provided betWeen the distributor and
Solid. This change takes place more rapidly at the inlet to the pump 53 to prevent the distributor
40 from becoming clogged. With irsolubie Sulphur.
an elevated temperature and one can employ
temperatures between 35° C. and 70° C. As the Ehe dry insoluble sulphur product is removed
temperature is increased, a shorter time of re from the bottom Of the dirier through Screw Con
tention is required. veyor 5: While the vaporized carbon disulphide is
Since the carbon disulphide in tank 6 is at its collected and take of through line 58 to be coin
boiling point (46.6° C. to 55° C. depending on the dens?di ini condie Ser 33 aEnd collected in, a, Water
concentration of soluble Sulphur in the carbon sealed tank 6. From this tank the collected car
disulphide and the presSure maintained in the bon disulphide is forced by punp through line
System) this is a convenient place. 'o retain the 62 to be returned to the Washer 29 with carbon
product although the retention can be effected in di Sulphide from line 3 .
a separate vessel. In tank 6 a retention time of EacCammple
from an hour to 24 hours may be utilized but I In One operation, Sulphur was vaporized at the
prefer to retain the product for from 1 to 4 hours. late of 300 pounds per hour. Sulphur vapor was
The shortest period of retention is usually desir introduced through inlets A at a fairly high ve
able if a good yield of insoluble Sulphur is re 55 locity, about 100 feet per Second, onto the surface
quired for some reversion to the soluble form of the liquid carbon disulphide in the lower por
may occur. The product, after retention, is of tion of the baffled scrubbing tower , the sulphur
alaVerageSize of about two microns and is com being innediately quenched. The baffles in the
parable to the finest Sulphur produced by special, tOWer Were. So arranged that the downcoming
expensive grindings or “micronizing' operations. 60 liquid carbon disulphide sprayed in through
The retention can also be practiced after the heads 24A and 26B kept the walls of the quench
product is removed from tank 6 and while the ing sections thoroughly washed with liquid car
product is in the form of a slurry. If the reten bon disulphide and prevented any sulphur par
tion at an elevated temperature is practiced on ticles from adhering to the walls of tower or
the final dry product a longer retention period 65 eScaping in the Vapors through line. 2.
is generally required. the actual quenching of the sulphur vapor
The Sulphur produced by the manner of op takes place in the absence of water, the water
eration. So far described is a mixture of soluble Seal on tank is being so arranged that water can
and insoluble Sulphur. However, because of its not enter the Scrubbing tower. Of the sulphur
finely divided form and physical characteristics, 70 produced in this operation, more than half was
it is useful as such, when separated from the in Soluble sulphur. This was separated from the
carbon disulphide, in place of those finely di Soluble Sulphur, pump 2's forcing the slurry into
vided sulphurs heretofore identified as flowers of the top of the washer 29, wherein the insoluble
sulphur manufactured by the various milling and Sulphur passed downwardly through the washer
grinding methods known in the art. against the countercurrent flow of carbon disul
 2.419:310
5 6
phide introduced at the bottom of the washer. and thus when it comes in contact with the insol
The washed insoluble sulphur-carbon disulphide uble Sulphur in the quenching chamber it Will
slurry was picked up from the conical bottom of contain no Water.
the washer 29 by pump 53 for discharge through PRODUCTION OFMIXTURES OFSOLUBLE AND
the distributor jets 54 to the drum drier 56. INSOIUBLE SULPHURS
EFFECT OF IRON AND OF WATER
When it is desired to utilize directly the sulphur
If tank 6 or any other portions of the equip produced by the quenching operation in tank 6,
ment include iron or mild Steel, considerable COr the discharge from pump 2 is taken off through
rosion may result if water is present, due to the O pipe f4 and is delivered directly into the header
interaction of the Water with the iron, carbon 54 on the drier 56 as in Figure 3. Any undis
disulphide and Sulphur to form iron Sulphide. tributed slurry is returned to the inlet of the
This formation of iron sulphide is accelerated by pump through line 42. The product removed
operating at the boiling point of carbon disul from the drum drier through the screw conveyor
phide and by the presence of Soluble Sulphur in 5 57 consists of a mixture of insoluble and soluble
the carbon disulphide. The presence of water Sulphur Substantially in the proportion in which
even as a sealing medium, as I have indicated in these are produced in tank 6. This product can
Figure 1, may therefore make the use of iron-free be used as such, the product being characterized
equipment desirable. The presence of iron sul by its fine, uniform yellow color and its extremely
phide in the insoluble sulphur is in any event 20 fine State of division, being of a size comparable
undesirable, since it discolors the product and has to that which can be produced only by special
an adverse effect on its stability. It has been milling operations.
found that the presence of very small amounts of INTENTIONAL REVERSION TO PROVIDE SOLUBLE
iron Sulphide and water in the insoluble Sulphur SULPHUR
accelerate the rate of reversion to the Soluble
form on heating. It is thus very desirable that 25 In case it is desired to have the product entirely
when the insoluble sulphur is Subjected to the Soluble in carbon disulphide, a small quantity
drying operation, the insoluble Sulphur or the of amnonia, can be introduced through line 43
slurry containing the insoluble Sulphur should into the outlet from screw conveyor 57 to mix
be as free as possible from iron Sulphide and 30 With the Sulphur and cause the insoluble to revert
Water. to the soluble form. The addition of any suitable
NSOLUBLE SULPEUR PRODUCTION alkaline material to the Sulphur will cause rever
sion of the insoluble sulphur to the soluble form
If a product having an initially high percent and annonium carbonate or other reversion
age of Sulphur insoluble in Carbon disulphide is agentS can be employed. It is also possible to
desired, of the order of 90% and higher, and if reWert the Sulphur by Wetting it. With a small quan
this product is to have only a low rate of rever tity of water before it is dried. Once the material
Sion to the Soluble form Under the most adverse is dry it is difficult to wet and is, in fact, more
conditions encountered in storage, I have found stable and reverts more slowly than does the
it highly desirable that the transformation of the 40, product made by extracting the soluble sulphur
Sulphur vapor to a finely divided solid form be pOrtion of flowers of sulphur With carbon disul
accomplished under Substantially anhydrous phide and like solvents.
conditions. If the liquid utilized to quench the The dry product from conveyor 5. can be wet
sulphur vapor is anhydrous, then the insoluble by bringing it into contact with water containing
sulphur product Will be quite stable, providing 5 a wetting agent or by first Wetting with methyl
contact with Water is not permitted until after or ethyl alcohol and then with water.
the material has been recovered and dried. In
Figure 2 I have shown the apparatus and System QUENCHING MEDIA
of Figure 1 modified by substitution for the water In place of carbon disulphide, one can use any
seals of a source of inert gaS 30 delivering gas non-aqueous medium which is non-reactive with
to a gasometer 3? and from this through gas Sulphur and Sulphur vapor under the conditions
header lines 32 to tank 6, washer 29, separator of quenching. The medium should preferably be
3S, tank 25 and separator 60. Thus the sulphur one which is a liquid at ordinary temperatures or
production occurs entirely in an anhydrous Sys Without application of high pressure. It should
tem, also be capable of taking up heat readily and
VVater haS a limited Solubility in carbon diSul quenching the Sulphur. Thus, one can employ
phide, about 0.14% (wt.) at 100°F. I have found benzene, toluene, or xylene. One can also employ
that if carbon disulphide Saturated With Water, petroleum hydrocarbon fractions of a suitable.
but not containing any entrained, Undissolved chemical nature so that they are not reactive
Water, is used as the reflux to the Scrubbing tower, 60 Under the conditions of quenching with the sul
good stable insoluble Sulphur may be produced. phur, Such as petroleum naphtha or kerosene.
This is due to the fact that sufficient heat is lib Pentane and butane can also be employed; how
erated in the quenching operation to vaporize. ever, the use of either of these would preferably
slightly more than two pounds of carbon disul require a System operating at a pressure above
phide per pound of Sulphur vapor quenched. This 65 atmospheric,
carbon disulphide Vapor passes up through the
scrubbing tower where it meets the downcoming STABILIZATION OF INSOLUBLE SULPHUR
carbon disulphide reflux containing the dissolved To reduce or prevent reversion of the insoluble
Water. As the carbon disulphide reflux is heated sulphur produced to the carbon disulphide form,
to the boiling point of carbon disulphide, all of 70 the product may be treated with a stabilizer;
the originally dissolved Water Will be Vaporized, usually a halogen. Such as iodine, bromine or
by virtue of the vapor pressure of water at the chlorine or a Sulphur-halogen such as one of the
boiling point of carbon disulphide. The carbon Sulphur chlorides or Sulphur bromides can be used.
disulphide reflux thus becomes completely an The quantity of halogen or Sulphur halogen re
hydrous as it passes down the scrubbing tower 5 quired is quite. Small and the treatment is there:
 2,419,310
7 8
fore easily effected. For example, a small quan Small quantity of a stabilizing agent, for ex
tity of halogen or sulphur halogen, 1% or even ample, sulphur monochloride, is fed into line if
less by weight of solution, can be included in the through line 4. In the second washer, the
carbon disulphide, or the atmosphere in drier 55 insoluble sülphur product is brought into inti
can carry the halogen. Since the halogens, par mate contact with the Sulphur monochloride,
ticularly chlorine and bromine, react readily with the sulphur product being maintained in the
sulphur to form sulphur halogens, these may be Washer for an adequate period of time to en
introduced either as the free halogen or Sulphur Sure the necessary contact and also to permit
halogen. These compounds are included herein the Stabilizer to be Washed out of the Sulphur.
and in the claims in the term halogen. 10 The treated stabilized sulphur, free of stabilizer,
Once the stabilization has been effected, the is removed from the bottom of the Washer T2
halogen or Sulphur halogen can be Washed out of through line 76, pump 77 forcing the Sulphur
the insoluble sulphur with carbon disulphide until Slurry through line 78 to a drun drier or other
none or only a minute trace remains without suitable recovery device.
reducing its stability. The use of the halogen, 5 The carbon disulphide containing Sulphur
particularly Sulphur Inonochloride or Sulphur monochloride is treated to recover the carbon
bromide, requires an anhydrous systein to avoid disulphide and the Sulphur monochloride. The
undue corrosion. In this case the Water layer liquid mixture is taken off through line 8 at
cannot be used and an inert gas such as carbon the top of Washer 72 and is delivered to a frac
dioxide is employed as in the flow sheet of Figure 2. tionating column f33. In this, the Sulphur
20 monochloride is separated from the carbon di
The naterial need not remain in the Sulphur after
it has been treated for stabilization but can be Sulphide, which is taken off as an overhead vapor
removed by Washing. through line 84 into a condenser 86 from which
As a stabilizer, the term. I apply to these ma it is delivered as a liquid through line 8 into
terials, one can use a halogen or a sulphur halo 25. a tank 88. In order to minimize the loss of
gen. Since the halogens, particularly chlorine CS2 and Sulphur monochloride by their reaction
to form carbon tetrachloride and Sulphur, frac
and bromine, react readily with sulphur to form tionating column 83 should preferably be a glass
a Sulphur halogen, it is difficult to say that one
and not the Other material is effective and I lined Wessel, Since iron Catalyzes the reaction
therefore include all such compounds in the term 30 to form carbon tetrachloride on heating. A
halogen. pump f 89 removes the recovered carbon disul
The action of the halogen or sulphur halogen phide through line 90 and delivers it through
is apparently to react with traces of water pres line 9 into the base of the washer 2. The
ent in the insoluble sulphur to be stabilized, Sulphur monochloride Separating in column 83
forming acidic materials such as hydrogen chlo 35 is removed through line 92 and is returned
ride which have been found to improve the Sul. through line A into the incoming stream of
phur Stability. The need for stabilization is sulphur-carbon disulphide delivered through line
reduced by carrying out operation in a complete . The carbon disulphide removed from
ly anhydrous System. Instead of a halogen or washer 29 is taken through line 20 into a frac
sulphur halogen other materials capable of tak 40 tionating column 2j 2 Wherein the carbon di
ing up the Water can be used. Materials can Sulphide is Separated from the Soluble sulphur
also be employed Which are capable of furnishing present, the latter collecting in re-boiler section
a halogen by hydrolysis upon contact with a 28 ?i, being removed as desired, through line: 206.
Water trace in the Sulphur. iitanium chloride The Overhead Stream of carbon disulphide
and bromide, thionyl chloride and phosphorous 45 vapor is removed through line 20 into a con
pentachloride and bromide can be used, although denser 21, the liquefied carbon disulphide pass
iron compounds should be avoided since ferric ing to drum. 22 from which it is removed through
chloride and other iron compounds cause re line 2:3 and pump 2 f4 for return through line
version rather than stabilization. These mate 26 to Washer. 29.
rials are essentially chlorine and bromine Sources. 50 GRANULAR SULPHUR
The stabilizing treatment of the insoluble sul
phur is preferably practiced after the insoluble If a halogen be present when the Sulphur vapor
sulphur has attained its hard, non-plastic, well is quenched in tank 6, a granular product is
dispersed condition. To accomplish this, the produced. The best description of this is that
stabilizing treatment is preferably practiced by 55 it is about the size and shape of corn which
bringing the halogen into contact With the Sul has been exploded by gently heating the corn
phur for the requisite period of time after it kernels until the corn "pops' and “pop-corn'
has been removed from tank 6, The time of results. Contrary to statements in the literature,
contact varies and is shorter the higher the Con quenching of the sulphur vapor in the presence
centration of Stabilizer in the Solution in Which 60 of a halogen does not improve the yield of carbon
the in Soluble Sulphur is Suspended as a slurry disulphide insoluble Sulphur or its stability.
and the higher the ternperature at Which the in In Case it is desired to produce a granular
soluble sulphur is stabilized. Retention of the Sulphur product, the halogen, or sulphur halogen
insoluble sulphur in suspension in a carbon di can be introduced With the Sulphur feed to the
sulphide Solution containing 1% of stabilizer for 65 Vaporizer. The carbon bisulphide Solution leav
1 hour at 90° to 100 F. has been found to ing the top of the Washer 29 will contain both
suffice. soluble Sulphur and the halogen or sulphur
STABILIZING OPERATION
halogen. This halogen or Sulphur halogen is
concentrated in the molten sulphur accumulated
Referring particularly to Figure 4, the insol 70 in the bottom of the fractionating tower 4? in
uble sulphur slurry from tank. 6 is introduced into Figure2.
washer 23 wherein it is Washed. With clean car The Soluble Sulphur returned to the melter
bon disulphide. The washed slurry is taken 44 through line 43 can carry a considerable por
through line 33 by pump 53 and is forced. Over. tion of the stabilizer, particularly when sul
through line 7 into a second washer 2. A 75 phur monochloride is employed. The stabilizer.
 2419310 10
sulphur mixture is then vaporized and fed into substantially all of the Sulphur to a Solid, and
? .. ? 9

the quenching vessel. This manner of Operation for Several hours.solid in contact With said liquid
maintaining said
is particularly effective in providing a granular 7. A process for production of sulphur com
product, prising quenching sulphur vapor by introducing
LOW TEMPERATURE WAPORIZATION a stream of said vapor into a body of an inert
non-aqueous liquid medium to remove from said
For operating reasons, it is sometimes desirable sulphur
to reduce the temperature at which the sulphur vapor stream sufficient heat to condense
is vaporized. In Figure 2 I have shown the Sul substantially all of the sulphur to a solid, said
phur vaporizer 6 as comprising a closed vessel 10 liquid being a solvent for only S lambda, and
maintaining said solid in contact with said liquid
202 fed with molten sulphur by line 29 from Sul
phur melter 44, and suitably heated to provide a for several hours.
stream of sulphur vapor for emission through prising 8. A process for production of Sulphur mu. Com
quenching sulphur vapor under Substan
line 4. Line 38 is extended by pipe 23 to deliver tially anhydrous
the quenching medium, such as carbon disul 5 liquid mediurn substantially conditions with a non-aqueous
phide, to the vaporizer, the quenching medium inert to Sulphur and
which, under the conditions of the quenching, is
being injected below the surface of the nolten vaporized
sulphur in the sulphur vaporizer. With Carbon to provide cooling for the sulphur vapor
disulphide present in the vaporizer, the Sulphur in carbon abisulphide,
and form finely divided solid sulphur insoluble
and recovering and drying
vaporization temperature can be lowered for ex 20 the finely divided solid sulphur under Substan
ample from 832°F. to 690° F., by vaporizing equal tially anhydrous conditions.
weights of carbon disulphide and sulphur, . The 9. A process for producing finely divided Sul
attack of Sulphur On the metal of Which the phur comprising discharging a stream of Sulphur
vaporizer is constructed is less when the Sulphur
is vaporized at a lower temperature. In addition 25 vapor into contact with a body of a non-aqueous
liquid inert to the sulphur to quench the Sulphur
a finer dispersion of the sulphur is obtained when and form a dispersion in said body of finely di
it is injected into this liquid carbon disulphide vided flocculent, plastic sulphur, maintaining Said
as a mixture with carbon disulphide vapor. sulphur dispersion in said body until said Sulphur
claim:
1. A process for production of Sulphur Com so
becomes well dispersed and non-plastic, and re
prising quenching sulphur vapor by introducing covering said Sulphur. -
a stream of sulphur vapor into a body of carbon 10. A process for producing finely divided Sul
disulphide to quench the sulphur and form finely phur comprising discharging a stream of Sulphur
vapor into contact with a body of a non-aqueous
divided Solid Sulphur in Said body, and recovering liquid inert to the sulphur to quench the Sulphur
said finely divided sulphur from said body. 35 and form a dispersion in said body of finely di
2. A process for production of S mu compris vided focculent, plastic sulphur, maintaining Said
ing quenching Sulphur vapor in a liquid inert to
sulphur and part of which is vaporized upon sulphur dispersion in said body for a period from
1 to about 24 hours, and then recovering Said
contact with the Sulphur vapor, collecting the
quenched sulphur in a body of said liquid, Said 40 Sulphur.
11. A process for producing finely divided sul
liquid being a solvent for only S lambda, remov phur comprising discharging a stream of Sulphur
ing the liquid containing the quenched Sulphur vapor into contact with a body of a non-aqueous
and recovering the S mu carried by the liquid. liquid inert to the sulphur to quench the Sulphur
3. A process for production Of S mu compris and form a dispersion in said body of finely di
ing quenching Sulphur vapor in a liquid inert to vided focculent, plastic sulphur, maintaining Said
Suiphur and part of which is vaporized upon sulphur dispersion in said body for a period of
contact with the sulphur vapor, collecting the about, 1 to 4 hours, and then recovering said
quenched sulphur in a body of said liquid to form Sulphur.
a slurry therewith, said liquid being a solvent for
only S lambda, removing the slurry containing 50 ing12.quenching
A process for production of Smu compris
sulphur vapor in a liquid inert to
the quenched sulphur and recovering the S mu sulphur and part of which is vaporized Upon Con
carried by the slurry. tact with the sulphur vapor, collecting the
4. A process for production of sulphur com quenched sulphur in a body of said liquid, said
prising quenching sulphur vapor by introducing liquid being a solvent for only S lambda, remov
a stream of said vapor into a body of carbon ing the liquid containing the quenched Sulphur,
disulphide to remove from said Sulphur vapor separating the S mul carried by the liquid and
stream sufficient heat, to condense substantially contacting the separated Snu. With a halogen to
all of the Sulphur, said carbon disulphide body remove water and stabilize the S mu against
being sufficient to dissolve the carbon disulphide
Soluble sulphur formed. 60 reversion.
5. A process for production of sulphur com 13. A process for production of Smu compris
prising quenching Sulphur Vapor by introducing ing quenching sulphur vapor in a liquid inert to
a stream of sulphur vapor into a body of a non sulphur and part of which is vaporized upon Con
aqueous liquid medium inert to the sulphur to tact with the sulphur vapor, collecting the
quench the sulphur, said liquid being vaporized 65 quenched sulphur in a body of said liquid to form
by the sulphur vapor introduced, and contacting a slurry therewith, said liquid being a solvent
additional liquid with said vaporized liquid to for only Slambda, removing the slurry containing
condense at least part of said vaporized liquid and the quenched sulphur, permitting Said Sulphur
Wash out any entrained sulphur in Said Vaporized to remain in contact with said liquid for at least
liquid. an hour, recovering the S mu carried by the
6. A process for production of sulphur com slurry, and contacting the recovered S mu with
prising quenching Sulphur vapor by introducing a halogen to stabilize the Smu against reversion.
a stream of said vapor into a body of an inert 14. A process for production of insoluble Sul
non-aqueous liquid medium to remove from Said phur comprising heating sulphur to provide a
Sulphur vapor stream sufficient heat to condense 75 vapor stream thereof, continuously introducing
 1.
2,419,810
said stream into contact with a volatile inert non
12
a queous liquid to quench the Vapor and form a vapor stream and quenching said stream with
solid Sulphur, recovering the quenched solid sul additional liquid to condense and Solidify the
phur from the liquid, and contacting the recoV sulphur mu as a finely divided solid, the liquid
ered Sulphur with a small quantity of a halogen. being a solvent for only Slambda.
15. A process for production of finely divided 21. Process for producing finely divided sul
sulphur mu comprising quenching sulphur vapor phur comprising contacting Sulphur in vapor form
With descending streams of an inert nonaqueous
by introducing into a stream of said vapor suffi liquid in sufficient quantities to condense substan
cient of an inert non-aqueous liquid medium to re tially all the sulphur to solid finely divided con
move from said Sulphur vapor strean Sufficient O dition and to form a slurry of said solid sulphur
heat to condense substantially all of the Sulphur, in Said liquid, and maintaining said sulphur sus
recovering the quenched, finely divided solid Sul pended in said liquid until the crystals thereof
phur nu, and Washing the recovered Sulphur mu becOme definite and nonplastic.
With a liquid carrying a quantity of a halogen sta 22. A process for producing S mu which com
bilizing S mu against reversion to S lambda. prises contacting Sulphur Vapors With a nonaque
16. A process for production of finely divided 15 Ous liquid which is a solvent for sulphur lambda,
Sulphur mu comprising quenching sulphur vapor at a temperature and in Such manner that finely
With a non-aqueous liquid medium substantially divided Solid sulphur is produced and a suspen
inert to Sulphur and Which, under the conditions Sion of said sulphur in said liquid is obtained,
of the quenching, is partially vaporized to provide 20 maintaining said sulphur in said suspension until
cooling for the sulphur vapor, recovering the a. Substantial Conversion into nonplastic crystals
quenched, finely divided solid sulphur mu, and of S mu occurs, and separating S mu from said
washing the recovered sulphur mu with a liquid liquid.
carrying a quantity of a halogen sufficient to 23. A process for producing sulphur which com
stabilize S mu against reversion to S lambda. 25 prises contacting Sulphur vapors with a nonaque
17. A process for production of finely divided Ous liquid which is a solvent for sulphur lambda,
Sulphur mu comprising quenching sulphur vapor at a temperature and in such manner that finely
With a non-aqueous liquid medium substantially divided solid Sulphur is produced and a suspen
inert to sulphur and which, under the conditions Sion of Said Sulphur in said liquid is obtained,
of the quenching, is partially vaporized to provide 30 maintaining said Sulphur in said suspension until
cooling for the sulphur vapor, recovering the a substantial conversion into nonplastic crystals
quenched, finely divided solid sulphur mu, and of Sulphur occurs, and Separating the sulphur
Washing the recovered sulphur mu with a liquid from Said liquid.
carrying a quantity of a halogen sufficient to 24. Process for producing sulphur in finely di
stabilize S mu against reversion to S lambda, 35 vided form comprising contacting sulphur in va
recovering the S mu and washing it with a halo por form with an inert nonaqueous liquid in suf
gen Solvent to rid the S mu of at least a sub ficient quantity to condense substantially all the
stantial portion of the halogen. Sulphur to Solid finely divided condition and form
18. A process for production of sulphur com a slurry of said solid Sulphur in said liquid, and
prising quenching sulphur vapor by introducing maintaining Said sulphur suspended in said liquid
into a stream of Said vapor sufficient of an inert 40 until the Crystals thereof become definite and
non-aqueous liquid medium to remove from said nonplastic.
Sulphur vapor stream sufficient heat to condense ARNOLD BELCHETZ.
substantially all of the sulphur and form a fioc
culent plastic sulphur product, and maintaining REFERENCES CITED
the Sulphur product at a temperature whereat
the product becomes a well dispersed, finely di The following references are of record in the
Wided non-plastic Sulphur. file of this patent:
19. A process for production of sulphur com FOREIGN PATENTS
prising Vaporizing Sulphur and a liquid to form 50 Number Country Date
a vapor stream, quenching said stream in a body 474,191
of Said liquid to form a slurry of solid sulphur British ------------- O??, 27, 1937
mu in said body, said liquid being a solvent for OTHER REFERENCES
Only Slambda.
20. A process for production of sulphur com Mellor, “Inorganic and Theoretical Chemistry,'
prising vaporizing Sulphur and a liquid to form Vol 10, pages 30, 31. Pub. by Longmans, Green
and Co., London (1930).