Reactor apparatus

An apparatus that comprises (a) a fluid-tightly closeable materials-treating or reaction chamber with at least its body portion substantially completely enclosed by a temperature-control fluid chamber provided by its being surrounded by a temperature-control fluid jacket, (b) means to rotate the jacketed chamber end over end about an axis substantially normally transverse to its central axis, (c) divider-baffling means dividing its temperature-control fluid chamber into a plurality of, such as four, substantially similar and independent control-fluid compartments or quadrants, (d) temperature-control fluid ingress means which enable feeding temperature-control fluid into such quadrant while the reactor is rotating, (e) means in each compartment or quadrant to affect the flow of fluids through it to provide substantially uniform overall heat transfer from each of them; and (f) fluid egress means to enable discharging heat-control fluid from these compartments during the rotation.

This invention is that of a materials-treating apparatus applicable as a 
temperature-controllable reactor, such as a pressure reactor as an 
autoclave, rotatable end over end about an axis normally transverse to its 
central axis and generally about midway of its ends. This apparatus is 
equipped with heat-control (i.e. heating or cooling) means for providing 
substantially overall uniform temperature through the treating chamber 
walls into its interior, and can include means enabling charging fluid 
material into the interior during operation. 
This apparatus enables conducting under selected temperature conditions and 
with agitation a chemical operation that has to be carried out with 
agitation under such temperature conditions. 
The treating apparatus or reactor of the invention can serve also as an end 
over end rotatable ball mill with or without pressure application and 
similarly as to heating or cooling control and/or fluid material during 
operation charging means, and having exceptional advantages over former 
ball mills rotatable about the central axis. 
An important feature of the invention is its steady provision of uniform 
overall temperature throughout its end over end rotation during its 
operation. 
Another feature of the apparatus of the invention is its avoidance of 
undesirable gas or vapor lock development in the heat-control means, with 
otherwise would prevent the provision of uniform temperature. 
A further feature of the apparatus is that in its use as a pressure reactor 
or autoclave, its end over end rotation provides the necessary agitation 
thereby eliminating the need not only for an internal shaft-driven 
agitator but also for a stuffing-box where such shaft enters an autoclave. 
Such stuffing-box has been a source of serious disadvantages because of 
its wear, leakage, maintenance and replacement cost, and limitation of the 
applicable pressures. 
Still another feature of one embodiment of the apparatus is its inclusion 
of means to enable feeding or, and even also, withdrawing liquid or other 
fluid materials into the reactor while it is rotating and even under 
superatmospheric internal pressure. 
Other features of the invention will be seen from its further description 
below. 
Broadly considered, the apparatus of the invention comprises (a) a 
fluid-tightly closeable materials-treating or reaction chamber with at 
least its body portion substantially completely enclosed by a 
temperature-control fluid chamber provided by its being surrounded by a 
temperature-control fluid jacket, (b) means to rotate the jacketed chamber 
end over end about an axis substantially normally transverse to its 
central axis, (c) divider-baffling means dividing its temperature-control 
fluid chamber into a plurality of, such as four, substantially similar and 
independent control-fluid compartments or quadrants, (d) 
temperature-control fluid ingress means which enable feeding 
temperature-control fluid into such quadrant while the reactor is 
rotating, (e) means in each compartment or quadrant to affect the flow of 
fluids through it to provide substantially uniform overall heat transfer 
from each of them; and (f) fluid egress means to enable discharging 
heat-control fluid from these compartments during the rotation.

The rotating materials-treating apparatus 10, e.g., reactor-autoclave or 
ball mill, of the invention, has (as FIGS. 1-3 and 6 show) its treating 
zone or reaction chamber 11 enclosed by the inner shell or cylindrical 
reaction chamber wall 12 with one outer end (upper as in FIGS. 1 and 3) 
tightly fitted into the inner circular wall of the circular opening of 
upper collar 14. The other end (lower as in the drawings) similarly is 
tightly fitted into the circular wall of the circular opening in lower 
collar 16. 
The reaction chamber is pressure-tightly closed by the upper cap 17 
removably secured to the outwardly extending annular flange 18 of collar 
14 by tightly securing means such as a sufficient number, e.g. 24, of 
securing bolts 19 extending through equally spaced apart bolt holes in cap 
17 and with their threaded ends tightly engaged in registry with the inner 
threads of correspondingly located bolt holes in flange 18. 
The lower end of chamber 11 similarly is closed off by corresponding lower 
cap 21 similarly secured to outwardly extending annular flange 22 of lower 
collar 16 by a corresponding series of bolts 23 extending through bolt 
holes 24 in cap 21, with their threaded outer ends tightly engaged in 
registry with the inner threads of the corresponding bolt holes 25 in 
flange 22. 
Wall 12 of treating zone 11 is encircled by a temperature-control fluid 
chamber 27 enclosed between that wall and temperature-control fluid 
chamber outer wall 28. The inner surfaces of the outer ends of wall 28, 
are pressure-tightly fitted over respectively the outer peripheral surface 
of annularly depending skirt 29 of collar 14 and the corresponding 
peripheral surface of upwardly extending annular skirt 31 of lower collar 
16. Those outer ends of wall 28 are fluid-tightly sealed by suitable means 
such as welding the circular part of each of them to the corresponding 
peripheral surface of each of skirt 29 and skirt 31. 
To enable rotating the reactor-autoclave or ball mill end over end, 
apparatus 10 (of FIGS. 1-6) is supported from bearings by sleeves about 
two rotatable diametrically opposed parts of a shaft 33 positioned with 
its axis of rotation running through the apparatus in a line substantially 
normally transversely to intersect the central axis. 
Each of these two separate parts 34 and 35 (FIG. 1) of shaft 33 has its 
inner and integrally attached (as by welding) to diametrically opposed 
locations longitudinally about midway along wall 12 of reaction chamber 
11. Each such shaft part is enclosed in and spaced away from its own 
respective temperature-control fluid sleeve 37 and 38 communicating with 
temperature-control fluid chamber 27. The outer end of each of these 
shaft-part sleeves or sleeve-jackets is liquid-tightly sealed off by its 
respective end or closure cap 39 and 40 with the outer end of each of 
shaft parts 34 and 35 respectively protruding in fluid-tight relationship 
(as by welding around their junction) through its respective cap. The 
inner end of each sleeve is integrally attached (as by welding) to jacket 
outer wall 28. 
Temperature-control fluid inlet 42 of stationary T-fitting 43 is mounted 
between two rotary unions 44 and 45 in shaft-part sleeve-jacket 37. Union 
44 pressure-tightly communicates between the T-fitting and the sealed off 
end of sleeve-jacket 37. Rotary union 45 similarly is connected between 
the T-fitting and inner end nipple 46, by which sleeve-jacket 37 is 
fluid-tightly and integrally attached to fluid chamber jacket 28. 
Sleeve-jacket 37 thereby communicates with chamber 27. 
On the other shaft-portion jacket 38, temperature-control fluid leaves it 
through outlet 47 in stationary T-fitting 48 is similarly mounted between 
two rotary unions 49 and 50. Rotary union 50 similarly is connected 
between T-fitting 48 and a second inner end nipple 51, by which 
shaft-portion jacket 38 is anchored to fluid chamber jacket 28 and 
communicates with chamber 27. 
The rotary unions should be such as stand up under the operating 
temperatures and pressures. Found to be very effective with this apparatus 
used as a rotating autoclave is the swivel joint illustrated (in cutaway) 
on the front cover (page 1) of the OPW Division of Dover Corporation, 
Cincinnati, Ohio, catalog and again on its page 3 which gives some detail 
illustrations and description and features of this rotary union. Other 
illustrations and more information on other models appear on page 9 of 
that catalog. Its page 2 shows that its models with stainless steel body, 
as used in this apparatus, are rated for pressures up to 1,000 psi (lbs. 
per square inch), and those with ductile iron body are rated for up to 600 
psi. Its page 12 gives pressure and temperature ranges graphs for them for 
their different body metals. Its page 15 lists over 200 gases, and 
inorganic and organic liquids and solutions with which they can be used. 
Apparatus 10 is mounted for rotation by rotatably supporting the 
diametrically opposed sleeve-nipples 46 and 51 in bearings 52 and 53 
respectively. However, when the apparatus is of such size or the strength 
of sleeves 46 and 51 and wall 28 are such that reinforcement is advisable, 
these sleeves can be reinforced by enclosing each of them in a separate 
trunion (not shown) snugly fitted over it and with the periphery of the 
inner end of such trunion welded to jacket wall 28. 
It is advantageous also to support the outer end of each shaft part 34 and 
35 in a bearing which conveniently can be branch arms 70 and 70a of 
bearings 52 and 53. A pulley 57 is mounted at the outer end of shaft part 
35, and for any larger size and heavier apparatus may be replaced by a 
sprocket or gear wheel to be driven by a chain belt, for rotating the 
apparatus. 
To distribute uniformly the temperature-control fluid to enable providing 
overall substantially uniform temperature through the entire treating or 
reaction chamber wall 12, temperature-control fluid chamber 27 is divided 
into four substantially similar quadrantal parts or quadrants. First 
chamber 27 is divided into approximately equal upper and lower halves by 
annular or peripheral baffle 60 encircling reaction chamber wall 12 and 
extending from it to temperature-control fluid chamber wall 28 in 
substantially fluid-tight engagement with them in a plane substantially 
normally transverse to the central axis of chamber 11 and running 
substantially through the axis of shaft 33. 
In this modification, annular or transverse baffle 60 passes at 
diametrically opposed locations through corresponding slots 62 and 63 in 
the inner ends of shaft portions 34 and 35 respectively. 
Each of these upper and lower halves of temperature-control fluid chamber 
27 then separately can be divided into substantially equal parts or 
quadrants (as seen in FIG. 1) by (i) the vertical divider baffles 65 and 
65a extending in substantially fluid-tight engagement with chamber wall 12 
and jacket wall 28 and between shaft part 34 and skirts 29 and 31 
respectively and (ii) divider baffles 66 and 66a in like engagement 
between walls 12 and 28 and shaft part 35 and skirts 29 and 31. 
To provide overall substantially uniform temperature distribution through 
the entire chamber wall 12, each such quadrantal portion or quadrant of 
temperature-control fluid chamber 27 includes at least one vertical and 
outer end shortened flow diverter baffle 68 as in the upper rear quadrant 
and like baffle 69 as in the lower rear quadrant (both as seen in FIG. 1), 
to promote serpentine stream flow of fluid separately in each of these 
quadrants. Each such short diverter baffle, as well as like baffles 68a 
and 69a (in the upper and lower front quadrants respectively, as seen in 
FIG. 3), extends also in liquid tight engagement from reactor chamber wall 
12 to fluid chamber wall 28. 
However, at its outer end (i.e. nearer a cap), each diverter baffle is cut 
off sufficiently to allow the stream flowing through its quadrant to pass 
almost completely and so extends, for example, roughly about 20% of the 
height of its quadrant short of cap 17 to provide a slot-like passage 71 
(FIG. 3) through which fluid can pass from one half (in FIG. 1 the right 
hand half) of the quadrant into its left hand half. The corresponding 
short diverter baffle 69 provides a corresponding passage 72 (FIG. 3). 
To avoid development of air or vapor lock in the innermost corner (near 
annular baffle 60, FIG. 1 center) when the heating fluid is a liquid, each 
of short diverter baffles 68 and 69, and also 68a and 69a, terminates 
about 3 to 4 percent of the quadrant height short of baffle 60 whereby a 
relatively small gas escape or vent orifice 73 and 74, and also 73a and 
74a, respectively is provided at each of such inner, or so-called 
equatorial, corners. The foregoing percentage figures for shortening the 
ends of the diverter baffles were used in an autoclave (of the invention) 
with a 54 inch axis length reaction chamber. 
In the modification shown in FIGS. 1-3 and 6 (e.g. of 17 inch inside 
diameter reaction chamber), the single short diverter baffle, such as 68 
and 69, in each quadrant is located at about midway between the full or 
divider baffles 65 and 66 and 65a and 66a respectively. However, in an 
apparatus of still larger capacity and thus correspondingly larger 
diameter, generally a larger odd number of diverter baffles, for example 
three, will be needed. 
In such case, i.e. using three intermediate or diverter baffles, they would 
be positioned parallel to one another as well as to divider baffles 65 and 
66 and at 30.degree. angularly separated locations around the periphery of 
chamber wall 12. However, with the larger number they should be positioned 
in staggered relation as to their respective terminations short of divider 
baffle 60. Thus, the larger or slit-like opening (e.g. 71) will be between 
the upper end of the first one of the three diverter baffles and the cap, 
below the lower end of the second one of them and transverse baffle 60, 
and again between the upper end of the third one of them and the cap; 
thereby to promote serpentine flow of the temperature-control fluid from 
its entry at the inner end of shaft part 34 into the quadrant and so on 
through it to its egress from the quadrant and on into the inner end of 
the shaft part 35. 
FABRICATING THE APATUS 
Cylindrical reaction chamber wall 12 may be prepared first. Annular baffle 
60 then is fitted over wall 12 at its required location and welded in 
place. Then collars 14 and 16 are fitted over its open outer ends and 
welded at least around the annular junction of the underside of the 
collars with the outer surface of wall 12. 
The various vertical baffles, e.g. 65, 66, 68, 69, 65a, 66a, 68a and 69a, 
are welded in place at their respective locations on the exterior of wall 
12. Shaft parts 34 and 35 then are placed diametrically opposite one 
another with their respective slotted ends 62 and 63 fitted over baffle 
60, and welded at their junctions with the latter and beyond the inner 
peripheral end of the shaft parts to the outer surface of wall 12. 
Two longitudinal half sections of chamber jacket wall 28 with cut out 
portions large enough to allow the shaft parts to protrude and jointly to 
provide circular openings spaced away from their inner ends are set in 
place around the outer surfaces of upper skirt 29 and lower skirt 31 and 
welded together along their longitudinal junction points and peripherally 
at their outer ends around the outer surfaces of skirts 29 and 31. 
The inner ends of nipples 46 and 51 are then inserted at their 
diametrically opposed openings in jacket wall 28 and welded around their 
peripheral junctions with the outer surface of that wall 28. Rotary unions 
45 and 50 then are liquid-tightly connected to the open outer ends of 
inner nipples 46 and 51 respectively. Then the inner end of each of 
stationary T-fittings 43 and 48 also is fluid-tightly connected with the 
outer end of the respective one of those two rotary unions. 
The inner ends of rotary unions 44 and 49 then are connected similarly 
respectively to the outer ends of the T-fittings. Closure caps 39 and 40, 
then held with the inner end of their skirt portions extended toward 
rotary unions 44 and 49, are slipped respectively over the outer ends of 
shaft-parts 34 and 35 to connect the inner ends of these skirt portions 
fluid-tightly separately to these rotary unions. The periphery of the 
orifice in the outer end of each cap, through which the outer end of the 
respective shaft-part still protrudes, then is welded to the shaft-part 
over their entire junction. Thereby the outer end of each of shaft-part 
jackets 37 and 38 is fluid-tightly sealed. 
The thus assembled rotatable reactor-autoclave then is mounted with nipples 
46 and 51 of its respectively opposed shaft-part jackets 37 and 38 seated 
in the pair of opposed bearings 52 and 53, and with the outer end of 
shaft-part 35 supported in bearing branch arm 70. Pulley 57 then is 
mounted and secured at the outer end of shaft-part 35 and connected by 
suitable belt to a driving source. Alternatively, pulley 57 may be 
replaced by a sprocket or gear wheel and connected by chain belt to a 
corresponding driving source. 
In addition to their effect on the course of the temperature-control fluid 
through temperature-control chamber 27, the various baffles advantageously 
strengthen not only that chamber but also the entire body portion of the 
end over end rotatable materials-treating apparatus. 
Continuous transverse baffle 60 and its connection with the separate 
shaft-parts is beneficial in the end over end rotation. Additional benefit 
in stabilizing the rotation stems from the support given to the pulley end 
of shaft-part 35 by branch arm 70 of bearing 53, and also by the support 
to shaft-part 34 by the corresponding branch 70a of bearing 52. 
The embodiment of FIGS. 1-3, used in the shortly below illustrative 
examples of use of the apparatus, has a reaction chamber volume of about 
58 gallons, one inch separation between walls 12 and 28; one-half inch 
thickness of baffles and of wall 12, one inch vent gap between transverse 
baffle 60 and the diverter baffles and four inch long slip-gap passage 
between them and the inner end of the skirt of the collars; two inch 
diameter shaft-parts, two and three-quarters inches inside diameter of 
their sleeve-jackets, one-half inch thickness of the jacket walls and 
one-quarter inch for wall 28. The closure caps are two inches thick to 
withstand 500 psi, and the bolt shanks have one and a quarter inch 
diameter. 
OPERATION OF APATUS 
The apparatus of the invention enables conducting under selected 
temperature conditions and with agitation a chemical operation which 
includes agitating a liquid phase and under selected temperature 
conditions, by enclosing whatever starting materials are involved in said 
operation in a liquid-tightly enclosed cylindrical operating zone by a 
liquid-tightly closeable zone-enclosure which enclosure is a heat 
conductor and has a greater axial length than diameter and is 
substantially completely enveloped by a temperature-control 
fluid-confining zone divided into a plurality of substantially equal 
control-fluid zonal parts; and agitating said operating zone contents by 
rotating said enclosed operating zone jointly with said fluid-confining 
zone end over end about an axis substantially perpendicular to and 
intersecting its longitudinal axis generally about midway between its 
ends, while running temperature-control fluid separately through each of 
said zonal parts under substantially identical flow pattern to provide 
substantially uniform overall indirect heat transfer between said fluid 
and said operating zone contents. 
This apparatus is applicable to any type of chemical operation including 
agitating a liquid phase under selected temperature conditions, whether 
the operation is merely a single step operation such as acting on one or 
more chemical substances, or a polymerization, or a step in a multi-step 
chemical procedure, for example, a chemical reaction between a plurality 
of substances or dissolving or otherwise dispersing one or more substances 
in a solvent or in a liquid vehicle as by use of some surfactant or 
emulsifying agent, or impregnation of a fluid (gas, vapor, or liquid) into 
a soft or hard solid substance, or solvent extraction or removal of a 
surface coating. 
EXAMPLE 1 
A suitable circular gasket was placed over the annular portion of cap 21 
and both were liquid-tightly bolted to flange 22. Reaction chamber 11 (54 
inches length and 17 inches inside diameter) was charged with the 
following materials in parts by weight to fill the chamber to about its 
full capacity: 
______________________________________ 
styrene monomer 40 parts 
stearyl methacrylate 3 parts 
isobutyl methacrylate 
8 parts 
ethyl acrylate 3 parts 
`360` aliphatic solvent 
30 parts 
diacetone alcohol 5 parts 
4-methoxy-4-methyl-pentanone-2 
5 parts 
`Cyclosol No. 53` (Shell Oil Co.) 
5 parts 
azo-bis-isobutyronitrile 
0.6 part 
benzoyl peroxide 0.2 part 
trinonyl phosphite 0.1 part 
di-tertiary-butyl catechol 
0.1 part 
______________________________________ 
Top cap 17 together with a suitable gasket was liquid-tigthly bolted to 
collar 14. 
Hot water from a water heater was fed through a connecting hose (not shown) 
to inlet branch 42 of T-fitting 43 at a temperature to provide to the 
reaction chamber contents a temperature of 155.degree. F., with the 
reactor rotating at 3.5 revolutions per minute. The water flowed through 
shaft-part sleeve 37 around shaft part 34 to the ingress to 
temperature-control liquid chamber 27 at the inner end of nipple 46. There 
it divided into four separate streams, one flowing into each of the four 
different quadrants of chamber 27 wherein each stream followed in its 
quadrant a course such as that now to be described in relation to the 
upper quadrant of the apparatus as viewed in FIG. 1. 
The bulk of the hot water flowed inwardly along the upper surface of baffle 
60 and upwardly between the opposed surfaces of divider baffle 65 and 
diverter baffle 68 and then flowed around the outer end of baffle 68 
through passage 71 and into and through the portion of that quadrant 
between the opposed surfaces of diverter baffle 68 and divider baffle 66. 
At the same time, a considerably smaller portion of the water in the 
initial part of the quadrant ran transversely and in part along the 
surface of transverse baffle 60 and on through escape orifice 73 into the 
second part of the quadrant, and there mingled with the water flowing 
toward baffle 60, and then out with it into the discharge space between 
shaft part 35 and sleeve 38, and out through outlet branch 47 of T-fitting 
48 and through a connecting discharge return flow hose to the water heater 
(both not shown). 
As the apparatus was rotating during this just described flow pattern of 
the heating water through the upper quadrant of the apparatus (as seen in 
FIG. 1), each of the other three streams of the incoming heating water 
flowing at the same time into its respective one of the other three 
quadrants followed a like pattern through the two separate parts of its 
quadrant, and on to discharge from it about the inner end of shaft part 
35, through the discharge passage around that shaft part to outlet branch 
47 of T-fitting 48 and on to the water heater. 
Rotation of the reactor continued at the same rate as the hot water was 
supplied to maintain the reaction contents at 155.degree. F. for 16 hours. 
Then the water was shut off and the rotation stopped. With the apparatus 
in upright position, a release valve (not shown) in the top cap was opened 
sufficiently (to a crack) to allow entry of air. Opening a discharge valve 
(not shown) in the bottom cap allowed the completed reaction mixture to 
run out into suitable containers. 
The product is a valuable resin polymer solution compatibly mixable in 
about one to one ratio with currently used drying oils such as tung oil 
and the like, singly or admixed, in the so-called over-coat varnish 
formulations to provide such an over-coat varnish to be applied over 
colored printing on papers such as on label papers. When dry, by 
evaporation of its solvents, this resin coating leaves over the paper a 
high gloss, adherent coating transparent to the various colored label 
printing. 
EXAMPLE 2 
Pigmented Suspension 
The shortly above-described operation was repeated with the following 
changes: 
The respective parts of each of the styrene monomer, stearyl methacrylate, 
isobutyl methacrylate, and ethyl acrylate were cut in half and the omitted 
quantities replaced by 27 parts of titanium oxide pigment by weight. 
Before charging the various chemical substances into the apparatus, a 
layer of ball mill flint pebbles (about three-quarter inch diameter size) 
were loaded into it to a depth of about 6 inches. 
The operation then was repeated as described above with end over end 
rotation for 12 hours. The product obtained at the end of that time was a 
very stable coating composition with exceptional spreadability, hiding 
power and covering; excellent adhesion, advantageous salt-spray 
resistance, and unusual dispersion in spite of its being ready for use 
without having been subjected to any kind of paint grinding mill 
treatment. 
MODIFICATIONS OF APATUS 
Instead of constructing the rotatable ball mill autoclave with a collar and 
removable cap at each end (as in FIGS. 1-3), it is built with each of 
reaction chamber wall 12 and temperature-control fluid chamber wall 28 
respectively having an integral rounded head as shown in FIG. 6. In this 
modification, the respective members of each of the pairs of vertical 
divider baffles 65 and 66 and 65a and 66a are continuous and unitary with 
one another in each pair. However, each of the diverter baffles, as 68, 
69, 68a and 69a still has its outer end spaced away from the continuous 
divider baffle to retain the slot-shaped passages 71 and 72, and also is 
spaced away from baffle 60 to provide the escape orifices 73 and 74; and 
if each quadrant has more than one diverter baffle, they are staggered as 
earlier described to provide serpentine flow. 
Both ends of the rotary autoclave can be made with such integral dished 
head at the outer ends of reactor chamber wall 12 as well as of chamber 
jacket wall 28. Also, the jacketed head at either end or both ends can be 
made with an openable or removable liquid-tightly closeable manhole (not 
shown), and with a pressure release valve as well as a safety valve and/or 
a liquid or free-flowing finely divided solids inlet valve and 
corresponding liquid or fluid mixture outlet valve in the other head. 
In some uses of the rotatable autoclave and/or ball mill of the invention, 
it may be necessary during the operation at high pressure and while 
rotating, to feed into the reaction chamber an additional reactant at some 
particular stage of the operation. That can be done by modifying one of 
the shaft parts, for example, 34 (as in FIG. 4), by providing in it a 
liquid passage bore 75 extending co-axially centrally through it from its 
outer end to, and with its inner end extending through and terminating at, 
the inner surface of the reaction chamber wall 12 to communicate with 
chamber 11. 
In that case, the bore terminates at its outer end in a fitting 
pressure-tightly connected with a rotary, i.e., rotatable union or joint 
connected to a feed line bringing in under pressure the reagent to be 
added. The inner end of bore 75 is fitted with a ball check valve with its 
valve seat 76, sealing ball 77 biased against the spring and so on valve 
nut 78 having one or more sluice-ways 79 inclining inwardly into the inlet 
end of bore 75, through which the reactant can enter reaction chamber 11. 
Upon supplying the reagent under a pressure greater than that in chamber 11 
thereby ball 77 is forced away from its sent to compress the spring and 
allow the reactant to pass on into the reaction chamber. When the needed 
quantity of reactant has been added, closing a feed valve (not shown) in 
its supply line and opening a release valve (not shown) between the feed 
valve and bore 75 allows ball 77 to be forced back by the spring as well 
as the pressure in reaction chamber 11 to its seat to close the ball check 
valve. 
Tool-engaging slots 81 and 82, in valve seat 76 and valve nut 78 
respectively, enable engaging and removing each of them with a tool for 
that use to allow cleaning out the check valve and, when necessary, bore 
75. 
The means for feeding temperature-control fluid to, and for its egress 
from, the separate compartments of the temperature-control fluid chamber 
of the embodiment of FIGS. 1-3, 5 and 6 can be modified by replacing shaft 
part 34 and its surrounding temperature-control sleeve 37 simply by the 
advantageous combination of a hollow shaft part 91 and a rotary (i.e., 
rotatable) joint 92 (as in FIGS. 7 and 9), and doing likewise as to shaft 
part 35 and its sleeve 38. As each such replacement is the same as the 
other, their details can be described by reference to one of them as shown 
in those figures. 
In them, the inner end of hollow shaft part 91 extends snugly through a 
peripherally fitting opening in fluid chamber wall 28 to, and is 
integrally attached (as by welding) to, the outer surface of reaction 
chamber wall 12. Wall 28 is fluid-tightly sealed (as by welding) around 
its peripheral contact with shaft part 91. The latter is hollow by having 
a central bore 83 (e.g., of 1 inch diameter in a 2 inch diameter shaft) 
extending longitudinally coaxially through it from its outer end to its 
inner end part within chamber 27. 
There bore 83 communicates with each quadrant of chamber 27 through a 
suitably sized circular orifice 84 (e.g., 0.5 inch diameter) to enable the 
respective portion of the temperature-control fluid to flow into its own 
quadrant. The central axis of each of such four orifices can lie on a line 
45.degree. from the vertical. The inner end of each shaft part can be 
slotted as at 62 and 63 of FIG. 1, or can terminate butt end against wall 
12 with the peripheral baffle 60 cut into two separate parts 62a and 62b 
(as seen in FIG. 8). 
The outer end of bore 83 is threaded to receive in fluid-tight registry the 
external threads at the outer end of the bore-engaging nipple 85 of rotary 
joint 92 whose fluid intake 80 is connected (in manner similar to fluid 
inlet 42 of T-fitting 43 of FIG. 1). 
In manner similar to that described for the temperature-control fluid flow 
through the embodiment shown in FIG. 1, the fluid leaving chamber 27 
enters the corresponding orifices into the bore of a diametrically opposed 
like combination of hollow shaft part and rotary joint and leaves its 
fluid outlet, for example, to return to a fluid heater. 
Any suitable fluid-tight rotary joint 92 can be used such as that available 
over the past 15 years as the Phillips EXACTO flexible rotary joint, 
packless and self-lubricated, produced by Phillips Company, Inc., of 
Ridgefield, New Jersey, and shown in gray on the front of their single 
sheet two page technical description (with red background for the upper 
half of its front page and black for its lower half). 
The hollow shaft parts of FIGS. 7 and 8 can be combined with means as shown 
in FIG. 4 for feeding fluid material into reaction chamber 11. Such 
combination is illustrated in FIG. 9. In it a fluid materials conduit 86 
extends longitudinally coaxially through, and spaced away from the inner 
wall of hollow shaft part 91, to leave a temperature-control fluid passage 
87 between them. 
Fluid materials conduit 86, fitted at its inner end with a ball check valve 
of the same construction and operation as that shown in FIG. 4 and 
described earlier above, similarly communicates (FIG. 9 with similarly 
numbered parts as in FIG. 4) with reaction chamber 11 to allow charging 
fluid material into it during the materials-treating operation therein. 
The inner wall of the outer end of each of hollow shaft part 91 and fluid 
materials conduit 86 is threaded to engage respectively in fluid-tight and 
pressure-tight registry with corresponding concentric engaging nipples 88 
and 89 of concentrically-dual-flow rotary joint 90 (shown without more 
detail in FIG. 9 because its details are not part of the invention). 
A suitable concentrically-dual-flow rotary joint effective in the foregoing 
combination is seen in catalog No. 14 of Rotherm Engineering Company, 
Inc., of Chicago, Illinois, such as its type YX of its pages 1-2 or type 
AR on its page 3. The temperature-control fluid enters through the inlet 
for it into fluid passage 87 and on through it and orifices 84 and heat 
control chamber 27 and so on out of the outlets from its quadrants and 
through like orifices 84 into a second egress combination such as that of 
FIG. 9 and through its temperature-control fluid egress passage and on out 
through the outlet for it in the rotary joint. 
In this second combination, the ball check valve in the inner end of the 
equivalent of the fluid materials conduit is modified so that the ball 
seat is between the ball and reaction chamber 11 and the spring is next 
beyond the ball in a direction away from the chamber. 
Thereby that conduit enables withdrawing reaction material from reactor 
chamber 11 at any point during the reaction period from the second outlet 
of the concentrically-dual-flow rotary joint, by proper sequential 
operation of hand operated valves (not shown) exterior of that second 
outlet. 
The apparatus of the invention can be made of ordinary high 
pressure-withstanding steel for all of its uses except those where contact 
with steel and any of its constituents at the operating temperature and 
conditions adversely affects the reaction products. For such uses reaction 
chamber wall 12 and the caps, whether removable or integral, can be made 
of stainless steel or be lined with it or some other suitable metal which 
does not adversely affect the materials being treated. 
While the temperature-control fluid chamber of the fully described 
illustrative embodiment of the end over end rotatable reactor of the 
invention advantageously is divided into four similar quadrants, the 
apparatus can be made with some other plurality of, even two, such 
substantially alike divisions or compartments of the control fluid 
chamber, so long as there is the same number of them above and below 
transverse or annular baffle 60, and an adequate arrangement of diverter 
baffles is used. 
For example, such reactor apparatus with only two like temperature-control 
fluid chambers lacks the vertical baffles 65, 65a, 66 and 66a, but 
includes the diverter baffles 68, 68a, 69 and 69a. 
It is advantageous as to the empty but closed apparatus, that its two 
halves resulting from dividing it by a plane running through the axis of 
its end over end rotation and the middle (of the thickness) of annular 
transverse baffle 60 be substantially equal in weight. 
GRINDING USE IN REACTOR, AND VARYING TEMPERATURE 
Many reactions using the apparatus as an autoclave can be carried out 
without including any ball mill-type metal balls or flint pebbles or 
stones such as used in Example 2 above, showing preparation of a pigmented 
polymer resin solution. While many reactions thus can be carried out 
without them, including grinding balls or flints is highly beneficial and 
advantageous where disaggregated solid materials are used, for example, 
for dispersing them in solvent or other liquid vehicles. 
The result is that such solid materials then not only readily are more 
finely divided so that they more readily are dissolved if they are soluble 
and need to be dissolved in the vehicle, or are more readily and very 
stably dispersed in the vehicle if insoluble in it; and that occurs 
unexpectedly in an inordinately shorter time than is possible in a ball 
mill rotating its usual longitudinally central axis or in grinding mills. 
After conducting any operation in the apparatus at elevated temperature, 
and so also at elevated pressure, or if a reaction requires cooling at 
some intermediate stage, the hot water or oil or steam supply to the 
temperature control fluid inlet 42 can be replaced by feeding cooling or 
cold water to it. That is done by suitable valve adjustments (not shown) 
ahead of inlet 42 to enable swiching from the hot fluid supply source to 
the cooling or cold water supply source. In that way after completing a 
run, the pressure in the reaction can be reduced to a suitable lower level 
or retained at some adequate level, for example, if desired to assist in 
discharging the contents which in turn can be cooled to any desired 
discharge temperature. 
Such possibility of cooling the reaction chamber is further advantageous by 
enabling using the apparatus as a ball mill for disintegrating and finely 
dividing materials which cannot be treated thus at ambient temperatures, 
but which are suitably frangible and non-adherent when cooled to some 
adequate temperature below ambient. 
While the pigmented suspension in Example 2 shows the reduction in size of 
its titanium dioxide pigment, that same pigment likewise can be reduced in 
size in other polymerization systems or other liquid systems. Other 
pigments likewise can be reduced in size in that specific or other 
polymerization systems or other liquid systems. Other solid particles in 
fluid systems, for example, solid adsorbing agents such as carbon black, 
or catalyst particles, similarly can be reduced in size either to provide 
additional contact surface or to present fresh surfaces such as fresh 
catalyst surfaces during the course of a catalyzed reaction. 
Use of the apparatus in an impregnation is illustrated by, but not 
restricted to, the following example: 
EXAMPLE 3 
Impregnation of Polystyrene Pellets to provide Expandable Polystyrene 
46 gallons (391 pounds) of water were charged into a 58 gallon stainless 
steel reactor apparatus as shown in FIGS. 1, 2 and 3 (having a 
longitudinal axis about three times its diameter). To the water there was 
added one pound of the "Gafac RE 610" anionic emulsifying agent, a 
phosphate ester of an ethoxylated alkyl phenol and composed of about equal 
parts of the mono- and di-ester and a maximum of up to 5% of nonionic 
component (product of General Aniline & Film Corporation, New York, N.Y., 
according to their patents 3,004,056 and 3,004,057); and a catalytic redox 
mixture of 25 grams of potassium persulfate and 10 grams of sodium 
bisulfite, with which mixture was included 10 grams of sodium 
pyrophosphate. 
Into that aqueous mixture there was charged 100 pounds of general purpose 
molding polystyrene pellets (3 millimeters size). More water was added to 
adjust the liquid level to leave sufficient room only for the addition of 
7 pounds of pentane, so that upon adding it the vessel was full to 
capacity. The impregnator then was pressure-tightly sealed by tightly 
bolting on its flat top cap over an intermediate gasket resistant to those 
liquids and their vapors. 
The impregnator then was rotated at 4 r.p.m. (thereby agitating the 
polystyrene pellets) while hot water was circulated through the 
impregnator jacket to bring the temperature of the contents to 195.degree. 
F. The heating was continued to keep the contents at that temperature for 
about 30 minutes. Then cooling water was circulated through the jacket to 
lower the temperature of the contents rapidly to about 100.degree. F. 
Rotation then was stopped, the impregnator opened and its contents 
discharged through a screen to let the water drain off, leaving behind the 
wholly free running, non-agglomerated pentane-impregnated pellets. These 
were rinsed lightly with tepid water to remove merely the water-soluble 
substances in the adhering suspending water, and then were air draft 
dried. 
Any other styrene-polymer can be impregnated similarly, as can also any 
other plastic or other material that is to be impregnated or leached and 
which physically can be handled in the reactor apparatus of the invention. 
The removable cap embodiment (FIGS. 1-3) of the invention is advantageous 
particularly for treating large bulky materials. 
The apparatus of the invention can be used in carrying out any other 
chemical operation, whether a chemical treatment or reaction, that has to 
be agitated under selected temperature conditions and at ambient 
atmospheric or other pressure. That is so also whether the treatment is to 
be carried out in solution form or in emulsion or liquid suspension 
vehicle or reaction medium, or whether including disintegrating and/or 
finely dividing in a liquid system a frangible material such as adsorbing 
agents, catalysts, liquid-soluble dye-stuffs, and insoluble pigments. 
Chemical synthesis is included in chemical reaction. The expression 
"chemical operation" is used generically to embrace all of these various 
treatments or reactions as described in this disclosure. 
By "body portion" of the apparatus is meant that part of it excluding the 
closure caps and any part of the collars exposed outside of wall 28 of the 
embodiment of FIGS. 1-3 and all of the embodiments represented by them 
when modified by the dished end of FIG. 6 excluding any valves in any 
manhole covers. 
Various other substitutions and modifications can be made in any of the 
hereinabove described apparatus embodiments of the invention and 
individual parts of it, within the scope of the appended claims, and which 
are intended also to cover equivalents of any of the specific embodiments.