US815761A - Glycerin-still. - Google Patents

Description

PATBNTED MAR-20, 1906. k

' GJSUDRE. LYGBRIN STIL OATION FILED mac W (T N 5.55 s. s

ATTO R N aYs pfiled by me'on as possible.

PATENT O ICE.

CHARLES- 'SUDRE, o F PARIS, FRANCE.

GLYCEFtlN-STIL L.

I Application filed DecemharIBO, 1902. $erial No. 137,127.

Specification of Letters Patent.

Patented March 20, 1906.

To all, whom it may concern: j Be it known that I, CHARLES SU RE, residing at 33 Boulevard Haussmann, Paris, in the Republic of France, have invented a certain new and useful Glycerin-Still and I do hereby declare the following to be a full, clear, and exact descriptionof the invention, suchas will enable others skilled in the art to which it appertains' to make and use the same. A divisional application of this case was January 6, 1904, Serial No. 187,931. Up 7 to the present in any apparatus or rocess for treating the residuary liquors rom alcohol distillation in order to extract from them glycerin andother useful products some mechanical apparatus forscraping or; cleaning the exhausted products has always had to be employed. By reason of the very; construction of anyprevious apparatus numerous accompaniments are produced which pass into the distilled liquid and render it very;

impure. It is well known that in order tof extract the glycerin without decompositionit is necessary to work in as complete a vacuum;

ter and a little glycerin, when, the material duces a froth and carriesfnumerous particles, which hinder the operations and in many off the processes used up to now render the working impossible if the dregs are viscous.

The apparatus which is the subject*of=the present application for a patent does away with this inconvenience. It is based on the following discoveries and appliances:

First. :If the vinasse' from a distillery (of "treacle,'for example) be distilled in a vacuum at a temperature of not' more'than 300, the

'residue after the-glycerin and the water have been "extractedisliquid at this temperature of "300 "and fiows away of its ownaccord. The glycerin and water are extracted in'a' time which depends on thethickness of the vinassaQ-My processconsists-in rinciple of providing along the walls of-an inc osure suit- "abl garranged," in which'there is a'vacuum an which is heatedfb some exterior source of heat in -such away that the temperature of 'thewalls "cannot-be greater than 300, a constant stream of :itli' 'vin asse' 'of regular and 5 5 regulated thickness: "Thus the vinasse 'en' The vinasse under the action of heat and in a vacuumfirst of all distilswa tersand pours awayin a continuous liquid state without. the intervention, of any me chanical apparatus and loses in its passage (supposingthat thisis of a lengthsuitable to the thickness of the liquid film) first of all its water and then its glycerin. t

Second. It is proved that if the vinasse is sufficiently acidulated the ammonia only escapes in infinitesimal proportions and remains concentrated in the'residue.

Third. By forcing the vapors to take up in the apparatus itself a rapid gyratory helicoidal movement I obtain by centrifugal force the impingement against the heated walls of the particles carried by the vapors, which distil anew;

Fourth. It isadmitted that it is necessary to have a current of superheated steam to help the distillation of the glycerin when the vinasse has become anhydrous.

v processes this steam is introduced from without, and thus dilutes the condensed mixture of water and glycerin. I utilize for this purpose the steam arising from the vinasse itself, which is superheated in the apparatus while taking up its gyratory .movement. The superheated steam then bathes and surrounds before'it leaves the apparatus the glycerin, which is given off by the anhydrous substance and draws it out of 1 These principles being setforth, I will describe as'a representative example a construction for the carrying out of the process shown ins'ection diagramatically in the accompanying drawing'and by which I put. these'princlplesxinto' practice but it is evi dent that'the forms may be infinitelyvaried.

"The apparatus is designed to be heated by too 1 coke or charcoal. I It consists of a distillingcolumn a,'formed of flangedcast ron tubes, three tosix meters high, according to the quantity of "water in the vinasse to betreated; Above this column is situated a 105 distributer. 1, which spreads throu han an} nular passage onto the interior wa ls of the 'columna' continuous stream of the vinasse to-be treated; At the footof this column is placed a pipe 2 for the escape of the gas and no In many On the contrary,

vaporswhich are given off by the vinasse under treatment. Below this the column is constricted and is terminated by a chamber 1), provided with stop-cocks c and d and in which the residue collects and which is arranged in such a Way that it can be drained off at regular intervals. Inside the column a is suspendedor fastened in any convenient way a rod f, round which'is coiled a helix 9, of which the outside surface is very close to the walls of the cast-iron column. The gas 7 and vapors escape into a shorter accessory column h, called the purifying-column, smaller than the principal column, but also containing a fixed helix. The solid substances drawn in impinge onto the walls and, distilling glycerin while descending the whole 7 length of the walls, enter a chamber like the V first, while the gas and purified vapor are directed into a condenser i by a suction-pump 7c. The whole is inclosed within a casing of V refractory material m, leaving sufficient space between it and the column for the passage of the gases for heating the apparatus. These gases are produced in a furnace n, placed outside the column. This furnace is fed by coke .or charcoal and is supplied with air by a blower 0. The hot gases proceed by a vertical flue p to the top of the casing inclosing the column. In their passage a second blower q injects cold air into them in a regulated quantity, so that their temperature at the top of the column is from 600 to 700 centigrade. Thegases redescend in contact with the cast-iron column and produce the evaporation of the water, whereby the greater portion of their heat is abstracted- About the middle of the column the gases are not more than 300. The small column h annexed. should not be higher than this point. As from other reasons the distillation of the rest of the glycerin, which is in very small quantities, requires very little heat, the temperature remains practically the same till it escapes by the lower flue.

The vinasse being watery and admitted to the vacuum, the Water contained is distilled at and in consequence until all the water is distilled the temperature of the vinasse scarcely rises above this in spite of the gases outside being at a temperature of 600 or .7.00 centigrade, all the heat of these being 7 used up to distil the water.

condenser connected. to said The steam produced. inside and at the top of the column exhausted by the suctionpump is required to descend, which it does by following the path of the helix, taking up a gyratory movement, which by the centrifugal force developed rids it of all the particles which are thrown against the wall, where the distillation is completed. While descending, the steam becomes superheated and helps in the distillation of the glycerin in the anhydrous portions.

Let us now follow an operation: The vinasse previously concentrated has some acid added to it, so as to corres 0nd to four or five per cent. of H SO T ien it is introduced into the top of the column, which has first of all been brought to the proper temperature by heating. The vinasse spreads in a film and submitted to heat in a vacuum undergoes a violent ebullition. It descends the length of the walls and loses first of all, as has been explained, its water and then. becoming superheated, its glycerin. The steam in the upper portion, which contains particles in suspension, enters the interior helix. The particles und er the action of centrifugal force are projected against the wall and further distilled and becoming heated surround and draw the escaped glycerin first into the accessory column h, Where it undergoes a fresh purification, then into the condenser, where it becomes liquid. The reslduary gases after havmg been drawn through the suction-pump are washed to rid them of any nitrogenous material they may contain, and then they escape into the at- V mosphere. The substances deposited in the accessory column undergo, as I have already described, a fresh distillation and the glycerin they distil merges into the glycerin-vapor from the principal column, which vapor passes through the accessory column. The

. substances deprived of glycerin flow into the bottom chamber, from whence by means of successive movements of the sto -cocks they are withdrawn at intervals. hus by this a paratus is obtained, first, a mixture of g ycerin and water of great purity, which has only to be concentrated to obtain glycerin ready for sale; second, a residuary liquid,

very hygrometric, which solidifies in air, retaining all potash and nitrogen, which can be sold as it is for manure or be redistillcd with lime to produce ammonia, methylamin, pyridic tars, or be treated in any other suitable manner.

I claim 1'. An apparatus for the purpose described comprising a vertical column, a stationary internal helix therein, a connected purifyin column at the side, a stationary helix in sald purifying-column, and a suction-pump and purifying-column, substantially as described.

2. An apparatus for the purpose described comprising a verticalcolumn having a cham- In testimony whereof I have hereunto set ber atthe bottom, a stationar internal helix my hand in the presence of two subscribing Io therein,asinallerpuiifying-co grnn afi the Sid? Witnesses. i

havin its ower en connecte to t e to 0 5 the fil st column, a stationary helix in Said CHARLES S I purifying-column, and a suctionump and Witnesses: condenser connected to said unfying-col v ANDRE MOSTIOKER, umn, substantiallyas described EDWARD P. MAQLEAN.

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