US82309A - Improvement in the manufacture of beomine feom bittern - Google Patents

Improvement in the manufacture of beomine feom bittern Download PDF

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US82309A
US82309A US82309DA US82309A US 82309 A US82309 A US 82309A US 82309D A US82309D A US 82309DA US 82309 A US82309 A US 82309A
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bromine
bittern
trough
improvement
steam
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/38Separation; Purification; Stabilisation; Use of additives
    • C07C17/383Separation; Purification; Stabilisation; Use of additives by distillation

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  • My invention is an improvement in'the process of extracting bromine from bittern or mother-water, and, in connection therewith, of an improvement in the apparatus employed for that purpose.
  • Figure 2 is a longitudinal sectional elevation thereof.
  • My improved apparatus consists-0f av trough or vessel, A, made of sandstone, and preferably of a single piece. It has a-cover, B, also of sandstone, made to t closely to the ⁇ top of the vessel A, and, when in use, luted down, so as to prevent the escape of ayof the bromine vapor.
  • a hole is bored at or near the bottom of .the vessel A, which hole is closedby la plug, D, when the apparatus is in use, and, when the operation is completed, the residual liquor is drawn oil' by removing the plug D.
  • a hole, C is bored longitudinally into the bottom of the trough A, from one side or end, extending toa point somewhere about the Amiddle of the vessel, andthen turning upwards, so as'to communicate' with the interior of the'trough.
  • the hole C may pass immediately through one of the walls of the trbugh, instead of extending through the bottom, although the method describodand shown in the drawing is preferablc,as itl admits the steam more centrally.
  • a steam-pipe, c through which steam passes from .a generator into the interior o f the trough A, is inserted linto or connected with the externalorilice of the bore C..
  • a small pipe, d is inserted into the topv ⁇ .of the receiver M, from which it conducts to a smaller vesselJ N, where' its orifice is sealed by immersion into an alkaline solution. This, however, is not a necessarypart-ofv the' apparatus.
  • the steam as it enters the trough, must force its way through the liquor, and, in so doing, it mixes intimately therewith, and produces a violent agitation of the particles of the uid, thereby eliminating the bromine moreeasily andrapidly, and causing it more freely to separate from the water and pass o, than it would do by the mere application of heat without the use of naked steam.
  • the bromi-nel' is eliminated in the form of vapor, it condenses in the worm, and iiows thence linto th'e receiver M.

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  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Description

G. A. H l lvIANN.A MANUPAGTURB 0F BRO NE FROM BITTBRN.
Nuzgaog.. Patented sept.22,'1868.
ww'w..
7 'AM' W nitrh tant atwt @Hire GrUS'IAV A. HAGEMANN, OF NATRONA, PENNSYLVANIA.
Letters Patent No.V 82,309., dated September 22, 1868.
IMPROVEMENT IN THB MANUFACTRB 0F BROMINE PROM BITTERN.
TO ALL WHOM I'I MAY CONCERN:
Be it known that I, GUs'rav A. HAGEMANN, a citizen ofthe Kingdomof Denmark, now resident at Natrona, in the county of Allegheny, and State of Pennsylvaniayhave invented a new and useful Improvement in the lldanufactureof Bromine; and I do hereby declare the following to be a full, clear, and exact description thereof,
My invention is an improvement in'the process of extracting bromine from bittern or mother-water, and, in connection therewith, of an improvement in the apparatus employed for that purpose.
In the accompanying drawing, which forms part of this specification- Figure 1 is a plan ortop'view of my improved apparatus, and
Figure 2 is a longitudinal sectional elevation thereof.
In both'gures, like letters of reference are employed to denote similar parts of the apparatus.
To enable others skilled in the art to make use .of my invention, I will proceed to describe my apparatus, and explain its use and operation. l
It is important, in the manufacture of bromine, to avoid the presence of metallic substances in the apparatus employed, because most of the metals. are attacked and .injuriously aected Vby theibromine, 4and also by the'muriatic acid whichis liberated during the process-of extracting bromine from thd'hittern. I
I have also discovered that the use of naked steam, introduced into the vessel containing the' mother-water l ,under treatment, eifects an important improvement in the processof extractinglthe bromine, aiding its evaporation, and facilitating as well as materially hastcning its elimination, not onlyby the physical action of the heat employed, but also by its mechanical elfect of agitating the particles of the liquor.
My improved apparatus consists-0f av trough or vessel, A, made of sandstone, and preferably of a single piece. It has a-cover, B, also of sandstone, made to t closely to the` top of the vessel A, and, when in use, luted down, so as to prevent the escape of ayof the bromine vapor. A hole is bored at or near the bottom of .the vessel A, which hole is closedby la plug, D, when the apparatus is in use, and, when the operation is completed, the residual liquor is drawn oil' by removing the plug D. A hole, C, is bored longitudinally into the bottom of the trough A, from one side or end, extending toa point somewhere about the Amiddle of the vessel, andthen turning upwards, so as'to communicate' with the interior of the'trough. The hole C may pass immediately through one of the walls of the trbugh, instead of extending through the bottom, although the method describodand shown in the drawing is preferablc,as itl admits the steam more centrally. A steam-pipe, c, through which steam passes from .a generator into the interior o f the trough A, is inserted linto or connected with the externalorilice of the bore C.. In the stone cover B'is a' small hole,.through which is inserted a glass tube, E, long enough to extend a few inches below the surface Adf the' fluid contents ofthe trough. Through a .larger opening in the cover B is inserted a stoneware funnel, theaseck of Vwhich also dips into the liquor under treatment. A leaden pipe, G, is fitted into thecover B, opening-'into the trough-'and serving as a gooslnedk,
fte carry ofi the bromine vapors. It terminates in a leaden worm, Lenclosed in,a"rfrigerating-vessel, H.. The
lower extremity of the worm I, passing out ofthe refrigerator H,-`enters a. receiver,'M,'wherein the'luid bromine is collected as it runs from the worm. The-joints around the glass pipe E, funnel F, and goose-neck G, in the ,listone cover B, are luted tight, so as to prevent leakage of brominevapr.- V
In order to permit of the escape of any air or-uncon'densed vapor, a small pipe, d, is inserted into the topv `.of the receiver M, from which it conducts to a smaller vesselJ N, where' its orifice is sealed by immersion into an alkaline solution. This, however, is not a necessarypart-ofv the' apparatus.
The operation of extracting bromine from mother-water, by means `of the apparatus just described, is as Vfollows l v The stone trough A is first heated by passing steam into it through thepipe c and bore C`.l The steam may be used at any convenient pressure, and need'not be much over 212 Fahrenheit. vWhenthe trough has been thoroughly heated, the mother-water or bittern, having been previously concentrated by boiling down, s run into the trough A, through the funnel F, until the vessel is about one-third full.
It is important to know 4the percentage of bromine contained in the bittern under treatment, asthe quanszene 2 -tityvof other ingredients employed in the process depends on the amount of brom'ine which is present. Y This is readily ascertained by analysis. To the bittern in the trough A, I then a'dd, through the funnel F, an amount of sulphuric acid which will be the equivalent of the-,quantity of bromine known to be in the quantity of motherwater to be treated. The acid vis first diluted with about four times 'its weight of waterl The trough is then filled up with mother-water until the mouth of the funnel F is covered with the iluid to the depth of a few inches. I then make a solution of chlorate of potash in water, or a thin pastelof black oxide of manganese and water or bittern, and add the solution or the paste (whichever may be used) slowly to the contents of the trough, through the glass tube E, which hasa funnel-shaped mouth for that purpose. The quantityof chlorate of potash, or of black oxide of manganese, will depend on the strengthpof the bromine in the bittern, being such as to be the equivalent of the sulphuric acid. When the liquor in .the trough A has been thus prepared, I turn on the live steam through the pipe and bore C, and the heat of the steam rapidly evaporates the bromine, as it vaporizes at about 142 Fahrenheit, much below the steam heat. The steam, as it enters the trough, must force its way through the liquor, and, in so doing, it mixes intimately therewith, and produces a violent agitation of the particles of the uid, thereby eliminating the bromine moreeasily andrapidly, and causing it more freely to separate from the water and pass o, than it would do by the mere application of heat without the use of naked steam. As the bromi-nel'is eliminated in the form of vapor, it condenses in the worm, and iiows thence linto th'e receiver M.
When the bromine ceases to iiow, the residual liquor is removed, as before stated, and the process is repeated with a fresh charge.
I am aware that sandstone troughs have been used before in making bromine, but always heated by a metallic pipe, or other metallic device, passing through the trough, so as to come'in* contact with the bromine and the liquor in the vessehwhich not only injures the bromine, but also rapidly destroys that part of the apparatus. These injurious effects are obviated in my apparatus; therefore,
What I claim as my invention, and desire to secure by Letters Patent, is-
1. The use, in the manufacture of bromine, of a sandstone trough or vessel, furnished with a bore, C, for the introduction of steam, so as to dispense with the insertion, into the lquor,'of metallic pipes.
2. Also, the use, in the process of extracting bromine from bittern or mother-water, of naked steam, introduced into the body of the liquor under treatment, for the purpose of combining the mechanical action of the steam with the physical eects of its heat, topproduce the desired eect.
In testimony whereof, I, the said GUS'TAV A. HAGEMANN, have hereunto set my hand.
G. A. HAGEMANN.'
Witnesses: v
ELL ToRRANcE, W. BAKEWELL.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2785052A (en) * 1951-06-22 1957-03-12 Metalectro Corp Production of hydrazine
US2917369A (en) * 1951-06-22 1959-12-15 Nat Distillers Chem Corp Production of hydrazine
US3642447A (en) * 1969-07-23 1972-02-15 Lynn Harold Hahn Bromine purification process by addition of steam to the vapor phase

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2785052A (en) * 1951-06-22 1957-03-12 Metalectro Corp Production of hydrazine
US2917369A (en) * 1951-06-22 1959-12-15 Nat Distillers Chem Corp Production of hydrazine
US3642447A (en) * 1969-07-23 1972-02-15 Lynn Harold Hahn Bromine purification process by addition of steam to the vapor phase

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