US1986165A - Distillation apparatus - Google Patents

Description

DISTILLATION APPARATUS Filed July 14, 1932 Patented Jan. 1935 William Sieck, Jr., Hubbard Woods, m, assignor to William Gan'ique & Company, Inc., Chicago,- IlL, a corporation of Illinois Application July 14, 1932, Serial No. 622,484

4 Claims.

A further object is to provide in an apparatus.

of this character a reflux column for the separation of the vapors, and which column is provided with means for regulating the temperature of the column, a condenserwith which the column is connected to eifect complete or partial condensa tion of the vapors leaving the column, and a steam ejector for maintaining a high vacuum in the entire system.

To the attainment of these ends and the accomplishment of other new and useful objects as will appear, the invention consists in the features of novelty in substantially the construction, 25 combination and arrangement of the several parts hereinafter more fully described and claimed and shown in the accompanying drawing illustrating this invention, and in which I The figure is a diagrammatic cross-sectional view of an apparatus of this character constructed in accordance with the principles of this invention. a

, Referring more particularly to the drawing, the

3 numeral 1 designates generally a still of any suitable material, fitted with a heating coil 2 into which latter steam, or a heating fluid, may be cessive resistance.

admitted through a valve 3 and, discharged through an outlet 4.

40 a discharge valve 6 for. removing the residue of the distillation, and is also provided with a perforated pipe 7 or a number of perforated pipes therein and near the bottom thereof, for the purpose of admitting steam directly into the mate-' rial to be distilled. The top of the still is fitted with a vapor outlet 8 which has communication with and extends to a separator 9. Theseparator preferably consists of a shell with a tangential inlet opening 8 through which thevapors from the still 1 are admitted.

Extending into the separator is an outlet pipe 10 which is preferably flared out at the lower end, and is covered at the lower end with a fine mesh screen or perforated metal disc 9 The still is provided with a fllling valve 5 and A drain pipe 11 leads from the bottom of the separator 9 to the still 1 and enters thestill, terminating at a point below the normal liquid level 48 in the still.

' The outlet pipe 10 which leads from the top of the separator communicates with aheat interchanger 12, preferably of a tubular 'typ'e, consisting of a casing 13 provided with tube sheets 14, into which latter are extended the ends of the tubes 15. The ends of these tubes open into two end compartments 69-70 arranged in the v heat interchanger so'that steam admitted through the opening19 into the compartment 70'will flow through the tubes 14 into the other compartment 69 and will pass out through-an opening 26. a

' The bottom of the'casing 13 is provided with a vapor outlet 16 which is connected to a reflux column 18 by means of a pipe 17. The outlet 19 I is connected to a desuperheater 21 by means of a pipe 20. The opening 26 of the heat interchanger 12 is provided with a pipe 27 leading therefrom a and communicating with the perforated pipe .7v

in the still. v Y The desuperheater 21 preferably consists 01. a closed tank with a perforated metal plate 22,,upon which latter is preferably placed suitable packing material 23, to constitute. extended surfaces for thedeposit of condensation and between which material the vapors and gases pass without ex- Steam enters the desuper-' heater through an inlet valve 24-and water en ters through a valve 25.

The column 18 is provided with a discharge "valve 28 to remove the finished product, and a heating coil 29 to which steam, or a heating fluid, may be admitted through a valve 30 and dis- 1 charged through an outlet 31.

The lower column tray 32 has in its centeria vapor opening 33 provided with an encompassing vertical rim or flange, and'with a drain pipe 34,.which latter extends toward and termi-' nates adjacent the bottom of the column. Perforated plates 35 are providedjand thereuponis placed suitable packing material 36, between which the vapors may pass. is provided with a vapor opening 38 encompassed by a vertical rim, and the column itself A-column tray 3'1 has adjac'ent'the tray an opening 39 to which is connected apipe 44 which has communicationwith a closed tank 42-. The pipe 44 is preferably provided with a valve 40, the opening of which valve allows theliquid in the tray to' drain into the tank 42. The liquid is removed from the tank 42 by means of a drain valve 43, and

a vacuum breaking valve 41. The numeral 45 represents a pipe for supplying water or any other liquid to the column, the supply of which is controlled by means of :avalve 46.

In order to obtain a good distribution of this water over the entire cross section of the column, the end of the pipe 45 is preferably fitted with a spray nozzle of any suitable construction.

Leading from the column 18 is a vapor outlet which has communication with a condenser 49,

- by means of 'a pipe 47. The condenser 49 is preferably of a tubular type consisting of a casing 51 provided with tube sheets through which are extended the ends of the tube 50, and through which latter the cooling medium flows, the vapors to be condensed passing around the outside thereof. The condenser is provided with a discharge valve 52 connected to a pipe 53,- which latter communicates with and extends, to a closed tank 54. The opening of the valve 52 allows condensates from the condenser 49 to flow into the tank 54 and are removed from the latter by means of a valve 55, and a vacuum breaker valve 56 may be provided.

The condenser 49 is connected to an ejector 60, preferably of the jet type, consisting of a throat member 58 and a steam nozzle 68, the flow of steam to the latter being controlled by a valve The discharge end of the ejector is connected to a condenser 64 preferably of the barometric type, consisting of a condensing chamber 62 and a barometric leg 65, terminating in a hot well 66. The condenser 64 is provided with a water supply pipe 63, and an outlet 61 leading from the condensing chamber and through which cut-- by means of the points of water ine vapors will let pipe air or other non-condensable gases may be removed by means of a vacuum pump (not shown) or any other suitable means. A description of the operation of the apparatus will be given in the distillationof glycerine, but

it is to be understood that it is not desired to.

be limited to this particular product, as other products may be distilled in the apparatus with equal efiiciency. The still 1 is filled to a level approximately indicated at 48, with crude glycerine, and steam is admitted to the coil 2. The steam ejector 60' is then set into operation, and the whole system is exhausted thereby to a vacuumof at least twenty-nine inches of mercury.

The steam valve 24 is gradually opened to admit steam into the desuperheater 21. Water is then admitted through the spray pipe by means of the valve 25, until the temperature of the steam leaving the desuperheater is that corresponding to a vacuum of about twenty to twenty-flve inches of mercury; Water will be evaporated or flashed into steam and this will withdraw enough heat from the live steam to reduce its temperature. The desuperheated steam flowsthrough the tubes of the heat interchanger 12 and finally through the'glycerine in the still pipes 27-7. The mixture of hot glycerine vapor and steam will pass upthrough the outlet pipe sand into the separator 9. Any

entrained liquids in the separator will be thrown or forced into the bottom of the separator and will drain or flow back into the still 1 through, the pipe 11, and the r the pipe 10 to the heat interchanger 12.

vapors will proceed through Due to the large diilerence in the boiling and glycerine, someof the glycerbe condensed in the heat interchanger 12, and will now in the form of a liquid,

1'7, together with the remaining vapors now containing a higher percentage of steam. By maintaining the proper temperature in the steam flowing through the tubes of the heat interchanger, the glycerine condensed at this point will be of high gravity and high purity.

At the same time the latent heat of condensation of the glycerine condensed in the heat interchanger 12 will be transferred to the desuperheated steam flowing through the tubes 15, resulting, in the superheating of the steam leaving the heat interchanger and entering the glycerine in the still 1' through the pipes 27 and perforated pipe '7. 5

The uncondensed glycerine vapors and steam pass up through the perforated plates 3735 and pervious pack-' ing material thereupon. Due to the reflux action of the plates and the pervious packing material each plate will accumulate a mixture of glycerine and water, and-the concentration of the glycerine in this mixture will vary on the different plates, being high on the lower plates and low on the upper plates, in fact if temperature and vacuum the reflux column 18 through.

conditions are properlyf controlled the upper plates will contain practically pure water.

Due to condensation of glycerine on the plates 35 37, and-on the pervious material, heat will be liberted, and unless this liberated heat is controlled, the temperature of the vapors and liquid in the column will rise, allowing glycerine vapors to reach the top of the column To prevent this, water is injected into the column by meansof the spray .water, upon flashing into steam, .will absorb heat and tend to cool the vapors passing to the'upper plates.

Vapor composition curves oi'- glycerine and water mixtures boiling under a high vacuum show the glycerine content of these. vapors to pipe 45, and which injected C. The introduction of water from, the spray and .its evaporation will tend to establish this condition on the upper plates and prevent loss of glycerine from the top of the column.

The water vapors and non-condensable gases leaving the column 18 pass through the tubular condenser 49 where condensed, depending on the temperature of the. cooling medium. I

The remaining water vapor and non-condensable gases will be removed by the ejector 60 to and the steam admitted to the elector will be condensed, and from which, the non-condensable gases are removed through the pipe 61 by means of ejectors or vacuum pumps (not shown).

The liquid dripping from the bottom plate 35 on to the tray 32 will be rich in-glycerine and will flow to the bottom section of the column throughthe pipe 34. Steam is admitted to the 001129, and the concentrated glycerine from the column and the interchanger is heated to boil oi! some of the water may be the condenser .62 in which latter the water vapors I the remaining water until proper concentration is reached. Any low boiling fractions will gradually collect on the tray 37, and will, from time to time, be drained to the pipe 44.

While the preferred method and apparatus for carrying this invention herein described, itis to ous changes may be in the steps of the method of into operationhave been be understood that variprocess, withinthe thetankflbymeansofmad e in thdapparatus and scope of the claims, without departing from the spirit of this invention.

What is claimed as new is:

1. A distilling apparatus embodying a still, a separator for receiving and separating from the vapors from the still foreign particles and entrained liquid in the vapors, a heat interchanger with which the separator is connected,

means for circulating a cooling fluid through the heat interchanger out of commingling relation with the vapors therein, the temperature of the cooling fluid being raised thereby, means for discharging the heated cooling fluid into the still, a reflux column, means for discharging the condensed and uncondensed vapors from the heat interchanger into the said reflux column, and means for discharging a cooling liquid into the said reflux column in commingling relation with the fluid therein to extract the remaining degree of heat by reducing the temperature causedby the condensation of the vapors.

2. A distilling apparatus embodying a still, a separator for receiving and separating from the vapors from the still foreign particles and entrained liquids in the vapors, a heat interchanger with which the separator is connected. means for circulating a cooling fluid through the heat interchanger out of 'commingling relation with the vapors therein, the temperature of the cooling fluid being raised thereby, means for discharging the heated cooling fluid into the still, a reflux column, means for discharging the condensed and uncondensed vapors from th; heat interchanger into the said reflux column, means for discharging a cooling liquid into the said reflux column in commingling relation with the fluid therein to extract remaining degree of heat by reducing the temperature caused by the condensation of the vapors, a condenser, means for passing vapors from the top of the reflux column into the condenser, and means for drawing any remaining vapors from said condenser.

3. A distilling apparatus embodying a still, 'a separator for receiving vapors from the still and for separating foreign particles and entrained liquid therefrom, a heat interchanger for receiv ing vapors from the separator, a reflux column for receiving condensed and uncondensed vapors from the heat interchanger, said heat interchanger embodying spaced chambers, passages forming communication between said chambers and constituting condensation surfaces, means forming communication between one of said chambers and said still, an additional chamber communicating with the other chamber in the heat interchanger, means for admitting liquid into the said additional chamber, and means for admitting aheating medium into the said additional chamber to flash the last said liquid into steam to be circulated through said heat interchanger and into the still.

.4. A distilling apparatus embodying a still, a separator for receiving vapors from the still and for separating foreign particles and entrained liquid therefrom, a heat interchanger for receiving vapors from the separator, a reflux column for receiving condensed and uncondensed vapors from the heat interchanger, said heat interchanger embodying spaced chambers, passages forming communication between said chambers and constituting condensation surfaces, means forming communication between one of said chambers and said still, an additional chamber communicating with the other chamber in the heat interchanger, means for admitting liquid into the said additional chamber, means for admitting a heating medium into the said additional chamber to flash the last said liquid into steam to be circulatedthrough said heat interchanger and into the still, and means individual to the last said liquid supplying means and the said heating medium for controlling them.

WILLIAM SIECK, JR.

CERTIFICATE OF CORRECTION.

Patent No. 1,986,165." .7 Januaryl. 1935.

4 mumsmcx, JR.

It is hereby certified that the name of the assignee in the above numbered patent was erroneously writtenand printed as "William Garrique & Company, Inc. whereas said name should have been written and printed as WilliamGarrigue 8: Company, Inc. as shown by the records of assignments in this office; and that the said Letters Patent should be read with this correction therein that the same may conform to the record of the case in the Patent Office. v

Signed and sealed this 19th day of February, A. I). 1935.

, I Leslie Frazer (Seal) Acting Commissioner of Patents.

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