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Publication numberUS1612167 A
Publication typeGrant
Publication dateDec 28, 1926
Filing dateMar 9, 1925
Priority dateMar 9, 1925
Publication numberUS 1612167 A, US 1612167A, US-A-1612167, US1612167 A, US1612167A
InventorsAlling P Beardsley, Carl E Mensing
Original AssigneeCalco Chemical Company
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Dinitrobenzene pellet
US 1612167 A
Abstract  available in
Previous page
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Claims  available in
Description  (OCR text may contain errors)

Dec. 28 1926. 1,612,167

A. P. BEARDSLEY ET AL DINITROBENZENE PELLET Filed March 9, 1925 I INVENTOR. 4/0/79 2 flea/"as/ey Patented ammo r. nnannsnn'r, or rLnInrrnLn,




Application filed Haircut, W25. Serial Ito. 1%,05131.

Dinitrobenzene has hitherto been placed on the market in the form of large blocksor lumps, or in the form of a rough granular material of irregular shape, size and fineness, which materials, when dry, generally include a large amount of dust. Dinitrobenzene is highly poisonous,- and either its vapor or its dust, when inhaled to any-appreciable extent, will seriously afiect workers employed in the manufacture or use thereof. Poisoning can readily be contracted by handling such material, containing fine particles and dust, and in breaking up large lumps for charging into vessels.

To minimize the harmful effects to workmen, when handling'such material, it has frequently been the practice to handle and ship dinitrobenzene in moist form. That is to say, during its process of manufacture,

it is made to contain sufiioient water to thinimize dusting. The 'use of water will unquestionably lessen the danger to workmen,

but it the material is left exposed for any appreciable time, the aqueous content will. evaporate and dusting will occur, resulting in the injurious effects referred to.

Moreover, when water is embodied in the commercial material it is usually not uni- 3 formly distributed and it is dcult to ob till tain a representative sample for the determination of moisture. It is therefore dificult to know how much actual dinitrob'enzene is contained'in a given weight of the moist material. I

ith these considerations in mind, the ob ject of: the present invention is to provide dinitrobenzene in convenient commercial form, in'order to permit it to be shipped and handled in a substantially dry state, without appreciable dusting, in such manner as not to render the workmen liable to poisonm Another object of the invention is to provide a simple, economical and eficient method whereby a new commercial form of material can beproduced.

Speaking-generally, the material of this invention consists of dinitrobenzene in pellet form, having a very close and marked resemblance to the small, smooth pebbles found in the beds of streams and in gravel pits. 7

Because of its form, we may figuratively refer to the material as dinitrobenzene pebbles.

A. characteristic feature of the material consists of the glazed surface of the pebbles which, in practice, may be made of a substantially uniform size, and with rounded or curvilinear exteriors, presenting no sharp points or edges and having a substantially uninterrupted smooth and lazed exterior. The glazed exterior and un roken'rounded surfaces edectually eliminate dusting of the material which would otherwise result from friction between them when they are handled in bulk. The rounded form of the material presents less surface than irregularly shaped grains of the same weight will have, and consequently less n naterial will volatilize from the surface.

can be practically and safely handled and shipped in a substantially dry condition, without being open to the well recognized disadvantages ot the commercial product now on the market.

lln practically carrying out the method of this invention in its preferred form, the dinitrobenzene' is subjected to a temperature above its melting point, and after being thereby transformed into a liquid, is passed through a progression of successively lower temperatures of a cooling fluid, for example, water. The drops or globules of dinitrobenzene are formed in water, the temperature ofwhich is at or above the meltin point of the dinitrobenzene, and thereafter such drops or globules are caused to gravitate through successively cooler re ions whereby they are solidified and forme into the pebble-like pellets desired. Having been thus formed and solidified, the pebbles are re moved from the water in which they were formed, and are dried, whereupon they are ready for shipment.

Features of the invention, other than those lhe material in the pebble form described adverted to, will be apparent from the hereinafter detailed description and claims, when read in conjunction with the accompanying drawings.

The accompanying drawing illustrates, 1n a diagrammatic manner, apparatus for carrying out the method of this invention but the showing therein made is to be understood as illustrative only, and not as defining the limits of the invention. In the diagrammatic showing, the apparatus is shown in central section.-

Referring to the drawings, 1 designates a relatively deep tank, provided near its top with a transverse partition 2, upwardly from the center of which extends a pipe 3, which extends as high as the annular wall at, and is open at the top. Also extending upwardly from the partition 2, and adjacent to the lateral wall of the tank is an annular wall 4,. which 1s coaxial with the pipe 3, and forms therewith an annular vessel 5. A pipe 6 leads through the top of the tank, and through this pipe the material to be treated is adapted to be discharged into vessel 5. The wall 4 is spaced from the side wall of the tank, and one branch 9 of a steam supply pipe 8 leads into the space thus provi ed. A second branch 7 of the steam supply pipe leads into the tank below the partition2. Also leading into the tank below the partition 2 is a pipe 10, to which is connects a box 21. Within the box 21, is an overflow pipe 12, which serves to maintain the level of the Water in the tank 1 approximately at the partition 2. The branch pipes 9 and 7 are provided with valves 13 and'14 respectively, and the pipe 10 with valve 16. Leading into the tank at or near the bottom is a pipe 17 to which is connected a cold water feed pipe 11, controlled by a valve 15. Also connected to pipe 17 is a drain pipe 23 controlled by a valve 18. At one side of the tank 1, near the bottom, is a manhole 19 normally sealed. In practice this is preferably positioned just above the partition 22.

In the lower part of tank 1, preferably close to the bottom is a partition 22. This partition is provided with openings and, if desired, is covered with a cloth whose weave is suited to prevent the passage of pellets of dinitrobenzene, while permitting the passage of water. In the cover of tank 1 is a vent 25,'which may be open to the atmosphere.

A portion of the partition forming the bottom of vessel 5 is provided with a number of nozzles 20, so formed and shaped as to function as droppers, so that material contained within the vessel may be discharged by gravity throu h the nozzles 20 in the form of drops or g obules.

In practice, the parts shown in the drawing may be made of any appropriate size,

and may be shaped differently or differently arranged from the specific showing made, but the construction illustrated diagrammatically shows a simple form of apparatus by which the method of this invention may be conveniently and economically carried out.

The specific method will now be described- The tank 1 is first filled with a liquid of less specific gravity than liquid dinitrobenzene. In practice, this liquid may vary, but we have found that water will give satisfactory results. This water is introduced into the apparatus of the drawing by closing the valve 18 and opening the valve 15, so that the water flows through pipes 11 and 17 into the tank. The tank is filled till the water overflows through pipe 10, box 21, and pipe 12. The valve 15 is then closed.

The valve 14 is then opened to permit the entrance of steam into the tank, for the purpose of heating the water or other liquid in the upper portion of the tank to a temperature at least as-high as the melting point of dinitrobenzene. After the desired temperature is attained, the valve 14 is closed. During this heating, excess water formed by-the condensation of steam can escape by pipe 10, box 21, and the pipe 12.

In practice the water at the top of the tank Will of course heat first. That is to say, the upper portion of the water will be the hottest, while the water at the bottom of the tank will be substantially cold. Between the partition 2and the bottom of the tank, the water will be of progressively lower temperature from the partition downward, and this condition may be figuratively referred to as a succession of progressively cooler regions in a downward direction.

After the Water in the vicinitv of the noz. zles has reached the desired temperature, dinitrobenzene, at a temperature to maintain it liquid, is fed through the pipe 6 into the starts to drip vessel 5 and immedlately throu h the nozzles 20 in the form of drops or glo ules. Steamis turned on at the valve 13 and this steam circulates about the wall 4 and in the head of the tank above the vessel 5, maintaining the dinitrobenzene in liquid form so that it may continue to drip through the nozzles.

Melted dinitrobenzene is of greater specific gravity than water, and will thus pass down through the nozzles slowly and form at the tips of the nozzles into drops, which, after being formed, will free themselves from the nozzles and drop through the water to the partition 22. It is of course essential to have the Water in the vicinity of the nozzles sufficiently hot to preclude any tendency for the material to solidify at the nozzles, and the temperature of the water is therefore kept sufficiently high to permit unrestricted formation of drops of substantially uniform size by turning on steam through valve 14. Should the temperature of the water near partition 2 be higher than desired, or should-the depth of the region of hot water in the top of tank 1 be deeper than desired, cold water nav be admitted through pipes 11 and 17, the displaced water overflowing through pipe 10, box 21v and pipe 12. I

As the drops leave the nozzles, and ravitate downward, they slowly pass t rough successively cooler regions of water, whereby they are cooled "and caused to solidify, the tankbeing sufiicicntly high to permit the solidification of the globules by the time they reach thepartition 22. They col-- lect on this partition as the process continues until a sufficient quantity is obtained, or until they have built up to such a height as to unduly decrease the distance between the nozzles and the accumulated product. At this point, steam is turned 0d at valve 14, if in use, and the hot water in the top of tank 1 is caused to overflow through pipe 12, by admitting cold waterthrough pipes 11 and 17. If desired, the "regions of hot water may be drawn oif by a valve suitably located in the side of tank 1, said valve being not shown in the drawing, but located just below the point where thewater'is of-a temperature which it would be undesirable to communicate to theaccumulated pellets.

The. drain valve 18 is then opened and the water in tank I allowed to run out through the partition 22.' If the hot water previouslyjn the top of tank 1 had not been first removed,.as just described, 'it'would finally reach the accumulated pebbles, as the water drained out through valve 18., and sinter them or melt them. When the water has been drained down below the level of partition 22, manhole 19 is removed, and the pebbles are taken out and either artificially dried or permitted to dry in the air. when the material is dried down to a moisture content of about one ortwo percent, it s in commercial form, as' it isthen approximately dry.

The finished product is found to be in the form of pellets, which closely resemble small pebbles, and are therefore fi urat-ively described. as dinitrobenzene pebb es. The individual pebbles have a lossy surface, and the contour of such pebbles is smooth and curvilinear. There are no' edges or corners, and the product of the operation is substantially uniform in size. The size of the pebbles is of course dependent u on the size of the drops formed at the nozz es. By controlling the head of liquid material above the nozzles and the specific gravit of the liquid in tank 1, and by suitable esign of the nozzle, the size ofthe finished pellets can be controlled within certain It will of course be understood that the specific gravity of the liquid contained in the tank below partition .2 will have an effectupon the size of the pebbles, in that the nearer the specific gravity of the liquid is to that of theliquid dinitrobenzene, the 7 larger will be the. pebbles, other factors such as temperature, liquid head and nozzle size being constant. \Ve have operated the apparatus with water, hose specific gravity had been raised by ac dition of other substances, with satisfactory results. Liquids other than water or water solutions may also be used. We have found however that water which minimizes volatilization of the material, when in the substantially dry condition to which we have referred.

Of'pronounced practical importance moreover is the fact that the material is converted by the method of this invention into a moresatisfactory commercial form, by a process whichv does not expose the workmen engaged in the carrying out of the process to the dangers heretofore often prevalent in the handling of dinitrobenzene such as breaking up and handling blocks of the solid material. The material passes into the apparatus through a pipe ,6 and is entirely enclosed during the-carrying out of the process in a closed chamber. When removed through the manhole, the-pellets have" acquired the smooth hard surface to which we have referred. The production of such material can be carried on with absolute safety to the workmen, as fumes and dust-. ing do not accompany the practising of the method, as is the case with the usual method of casting the material in molds and break- .i'ng it up.

The foregoing detailed description deals with the invention in its preferred practical form, but the invention is to be understood as fully commensurate with the appended claims;

The term dinitrobenzene, as used in the foregoing specifications, is understood to mean the commercial product usually described by this term, and which consists in a mixture of mta, ortho and para isomers.

Having thus fully described the invention, what we claim as new and desire to se-- cure by Letters Patent is: V '1'. As a new article of manufacture, dinitrobenzene pebbles having smooth glazed surfaces.

2. As a new article of manufacture, dinitrobenzene pebbles of smooth curvilinear trobenzene ebbles having smooth glazed contour and having lazed surfaces. surfaces and of not exceeding two percent 3. As a new artic e of manufacture, .dinimoisture content. trobenzene pebbles of approximately uni- In testimony whereof we have signed the 5 form size, each of which pebbles has a foregoing specification.

smooth glazed surface. ALLING P. BEARDSLEY.

4. As a new article of manufacture, dini- CARL E. MENSING.

Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US2471358 *Nov 22, 1946May 24, 1949Vernon V StephensonCapsulating method and apparatus
US2485249 *Feb 19, 1944Oct 18, 1949Davison Chemical CorpProcess and apparatus for manufacturing gels
US2557549 *Apr 9, 1948Jun 19, 1951Gasoline Res Ind & CommercialApparatus for the preparation of solids containing liquid hydrocarbons
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US3882208 *Sep 30, 1970May 6, 1975Us NavyMethod for production of spherical particles of a solid material
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US6223542Nov 30, 1999May 1, 2001Dippin' Dots, Inc.Cryogenic processor for liquid feed preparation of a free-flowing frozen product and method for freezing liquid composition
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U.S. Classification568/932, 264/14, 425/10, 264/3.5, 264/DIG.370
International ClassificationB01J19/24, B01J19/06, C07C205/06
Cooperative ClassificationB01J19/06, C07C205/06, B01J2219/00121, B01J19/24, Y10S264/37
European ClassificationB01J19/06, B01J19/24, C07C205/06