US1322757A

US1322757A - Method op and apparatus eor producing ammonium suleate

Info

Publication number: US1322757A
Authority: US
Publication date: 1919-11-25
Anticipated expiration: 1936-11-25

Description

H. A. CARPENTER.

METHOD OF-AND APPARATUS FOR PRODUCING AMMONIUM SULFATE.

APPLICATION FILED FEB. 15! I916.

1,322,?5Z Patented Nov. 25, 1919.

3 SHEETS-SHEET 1.

INVENTQR H. A. CARPENTER.

METHOD OF AND APPARATUS FOR PRODUCING AMMONIUM SULFATE.

APPLICATION FILED FEB. 15, 1916.

1,322,757 I Patented Nov. 25, 1919.

3 SHEETSSHEET Z.

mg. 2 I

WW I

H. A. CARPENTER. METHOD OF AND APPARATUS FOR PRODUCING IAMMONIIUM SULFATE.

APPLICATION FILED FEB. 15, 1916.

Lfi fifiih Patented Nov. 25, 1919.

3 SHEETS-SHEET 3.

INVENTOR the bath may TYMTED STATES @FFTQE.

HENRY A. CARPENTER, OF SEWICKLEY, PENNSYLVANIA, ASSIGN OR TO RITER-CONLEY MANUFACTURING COMPANY, OF PITTSBURGH, PENNSYLVANIA, A CORPORATION OF NEW JERSEY.

METHOD OF AND APPARATUS FOR PRODUCING AMMQNIUM SULFATE.

Specification of Letters Patent.

Application filed February 15, 1916. Serial No. 78,444.

To all whom it may concern:

Be it known that T, HENRY A. CARPENTER, a citizen of the United States, and resident of Sewickley, in the county of Allegheny and State of Pennsylvania, have invented certain new and useful Improvements in Methods of and Apparatus for Producing I Ammonium Sulfate, is a specification.

This invention relates to the production of sulfateof ammonia by subjecting coal gas to an acid saturation bath, the desired reaction of which the following resulting from contact of the ammonia ladengas with the sulfuric acid content 'of the bath.

One object is to providea controlled or predetermined uniform temperature condition within the saturator, and particularly at the gas outlet thereof, whereby the reaction is caused. to proceed under conditions most favorable for the production of high-grade sulfate, and whereby the temperature of the inlet as may be so regulated as to insure vaporization of water from the bath in desired .amount.

A further object is to utilize conditions inherent in the saturation bath for automatically controlling replenishment of the water and acid contents thereof, avoiding either over or under supply and maintaining a saturation bath of uniform volume and acidity. .The level of the bath is preferably utilized through the medium of a float for regulating the water additions, and the acid replenishment is determined by the specific gravity of the bath by means of a hydrometer.

Another object is to produce an acid-free sulfate, and this I accomplish by thoroughly washing the salt, waste" being revented by discharging the acid-carrying water into the saturator, and as the water which replenishes be used for this purpose, the desired conditions incident to the bath and its maintenance are in no way disturbed. The washing is made very effective by causing the Water to flow counter to and in contact with the sulfate as the latter is withdrawn from the saturator, whereby the sulfate is discharged free of acid.

Another object is to insure thorough and complete dissemination of the acid content throughout the saturation bath, the latter being usually about'a 5 %'solution. The addition of a small amount of acid of great concentration to the relatively large volume of the bath renders thorough mixing diliicult if not impossible if attempted in that zone or portion of the bath entered by the gas. To circumvent this unfavorable condition I maintain the bath in two bodies, with means for maintaining constant circulation between them. The reaction takes place in one of the bodies and the acid replenishment is accomplished in the other body, and by this means a thorough and uniform mixture is had, particularly in that portion of the bath where the reaction takes place.

In Figures 1 and 2 of the accompanying drawings apparatus for practising the invention is illustrated, the showing in both views being largely diagrammatic, Fig. 1 illustratipg the same primarily in side elevation with t 1e while in Fig. 2 the electrical circuits and connections are shown, together with a vertical section of the auxiliary saturator bath chamber. Fig. 3 is a detail of the mechanisms actuated by the float and hydrometer for eflecting the opening and closing of the circuits controlled thereby. Fig. 4 is a View in vertical section of the main saturator chamber together with a form of conveyer for removing the sulfate therefrom, and Fig. 5 is a sectional plan of a portion of the chamber, taken on line 55 of Fig. 4. Fig. 6 is a view in vertical section of part of the structure mounted on the saturation chamber for supporting and operating the conveyor, the

parts being illustrated at right angles to that shown in Fig. 4. Fig. 7 illustrates one of the conveyer buckets in detail.

Referring to the drawings, 2 designates the saturator, and 8 the pipe for admitting coal gas thereto, the gas passing into the upper compartment 4 of the saturator at the eXterior of the dome 5. Space etis in free communication with the jacket-like space 6, the latter being formed by the downward continuation 7 of dome 5 and the outer wall 8 of chamber 2. Space 6 is in open communication beneath the level of the bath with the interior of the saturation chamber. From the chamber-encircling space tithe gas is conducted into the hollow radially arranged distributin the level of the bat various electric connections omitted,.

Patented Nov. 25, 19-19.

tive distribution throughout all portions of the gas-entering Zone of the bath. The pres sure of gas is sufficient to depress the liquid level in space 6, so that the gas may freely enter distributers 9, as shown in Fig. 4. Upon emerging from the bath the gas ascends into dome 5 from which it passes through discharge pipe 11.

lt is desirable to regulate the temperature of the gas within the saturation cham ber. One object of such regulation to maintain the gas at an eflicient absorbing temperature, whereby the Water content of the bath will be depleted in such amount that the Water required to replenish the same will be sniiicient to thoroughly wash. the sulfate as it is withdrawn from the saturator, producing an acid-free salt. Another object of such regulation is to maintain. the temperature as low as is consistent with an efficient reaction, a better grade of sulfate being thus produced than when the temperature is excessive. A function of the saturator is availed of for accomplishing this automatic regulation, and in the preferred practice the temperature of the gas discharging from the saturator is thus utilized.

'In the embodiment of the tempe'ature regulation here shown, 15 designates a gas heater of usual construction through which a circulation of heated waste gases may be maintained by blower 16. The gas to be actuated by a thermostat 2% of suitable typeheated enters from a main 1? and discharges through pipe 18 into the saturator inlet 3. Extending around the heater from main 1.7 to inlet 3 is bypass l9, and controlling the flow to the heater and to the bypass is a damper 20 which is adapted to be actuated by an electric motor 21, which is by prefer- 'ence connected to a three-phase circuit 22 by a reversing switch 23 of familiar construction, and this switch is adapted to be having its terminal 25 entered in the saturator gas outlet 11. By this means both heated and relatively cool gas is passed to the saturator, the proportion of each being determined by damper 20 which, in turn,

is controlled automatically by the temperature at the saturator outlet, the reversing switch operating to actuate the motor in direction to admit more or less heated or cooled gas, or to remain inactive when the switch is in neutral position, all as determined by the movement emanating from thermostat 24.

The invention embodies automatic regulation for controlling the replenishment of the water and acid contents of the saturation bath, but before describing these features referent. will be made to the disposition of the bath in two separate bodies between which constant circulation of the liquid is maintained.

Upon referring to the drawings, it will portion of the bath that is required to be of maximum acidity, 2., the portion w th which the gas is in contact after discharg ing from battles 9. Also, with the circula tion outlc leading from the upper portion of the saturation bath there is practically no Withdrawal of sulfate into chamber 30. Circulation is maintained by means of a pump 36 driven by motor 37 and to which pipe 32 is connected, and by this means the contents of

chambers

2 and 30 are constantly mixing and interchanging.

The advantage of the foregoing arrangement results from the fact that the relatively small amount of acid of high concentration is supplied to chamber 30 and is thoroughly mixed with the saturation bath in said chamber and before reaching chamber 2., \Vhereas, if the acid were introduced directly into chamber 2 there would be no opportunity for obtaining a thorough mixing and to that extent the operation of the saturator would lack uniformity and its efficiency would be correspondingly lessened.

Functions of the saturation bath are utilized for automatically controlling the inflow of water and acid, whereby the volume and acidity of the bath are main tained substantially constant. The water supply may be obtained from a main. i0

which is adapted to discharge into the con veyer tube 41 (presently to described) extending downwardly into =ti .t open to the lower portion or 5-3 and and switch. By this means the flow of water through main 40 may be accurately controlled, motor at?) being controlled by the switch to either decrease or increase the flow or to maintain a predetermined con. stant flow, determined by the liquid level of chamber 30.

The supply of acid may be drawn from a suitable elevated container 50, a valve 51 controlling the flow therefrom into chamber A reversible electric motor 52 for actuating this valve is connected in circuit 22, the direction of themotor being controlled by a solenoid reversing switch conventionally shown at 53. This switch is under the com rol of hydrometer 5% located in chamber 30, the hydrometer stem 55 being movable through a vertical guide 56 carried by the float and at its upper end pivotally connected to one end of lever 57. This lever is mounted between its ends on fulcrum e7, being thus fulcrumed coincidentally with lever 526. the circuit extending to one side of switch is movably supported at 59 by lever 46, and said interruption is adapted to be closed by the bridging contact 60 carried by one leg of lever 57 when the hydrometer has risen sufficiently to effect such operation. A like interruption (51 in the branch of the circui extending to the other portion of switch .33 is movably carried by the opposite leg of lever t6, and is adapted to be closed by the bridging contact 62 movably carried by the portion of lever 57 that is distant from contact (30. As variations in the liquid level have substantially the same position-changing elfect on the float and hydrometer, levers l6 and 57 have substantially the same moven'ient on their common fulcrum 4:7 in resporse to such variations. This results in maintaining the circuit interruptions 58 and ($1 in substantially the same relation to contacts 0 and (32 irrespective of liquid level changes, and hence said parts are in proper relation for controlling the direction of motor 52 by movement [of the hydrometer relatively to the float, determined by the spe cific gravity of the bath. I

The quality of ammonium sulfate is frequently seriously impaired by the presence of sulfuric acid which is of a viscous nature and adheres to the salt in such manner that ts removal presents a difficult problem. Also the acid removed from the bath with the sulfate is an element of waste. The present invention provides for effectively washing the sulfate during its withdrawal from the saturator so that it is discharged from the apparatus in a non-acid state The means here shown for accomplishing this purpose consists of an endless conveyer chain (35 within tube 41 and carrying perforated or open mesh buckets 66. This conveyer is mounted in tube 41 on the upper and lower sprocket wheels 67 and 68, respectively, jUIH'LHlctl in the vertical parallel arms of a supporting frame. The upper end of this .l'rann comprises a spindle 70 that is rotatablev in bearings 71 of frame 72, the latlcr mounted on saturator 2, a motor 73 being eared to the spindle at 7 whereby the cndloss conveyor and its support are rotated about ,vertical axis without interfering An interruption 58 in the branch of thereof.

veyer support about its vertical axis operates to drive the upper sprocket, thereby keeping the conveyer in motion. Buckets 66 are thus caused to fill with sulfate at the lower end of tube 41 and discharge at the upper end of said tube.

The movement of the conveyer about a vertical axis combined with the vertical travel of the buckets results in so agitating sulfate at the lower end of tube tl as to maintain an ample supply Within-reach of the buckets atall times. 7 9 projecting laterally from the lower extremity of frame 69, Figs. 4c and 5, sweep through the sulfate as the frame is rotated, thus still further agitating the same. At the upper end of the conveyer the inflowing fresh water is discharged from pipe 40 through the ring or manifold 48 so that the sulfate is thoroughly washed while being. elevated through tube 41 and is freed of the acid adhering thereto, the water draining therefrom through the ascending perforated buckets.

It is characteristic of the cleansing operation that the sulfate and water move or flow in opposite directions through a common path of substantial length with the scrubbin action proceeding from end to end The sulfate encounters progressively clearer or fresher water as it moves toward the discharge end of the conveyer, whereby a most effective washing and rinsing action is had. \Vhile this contra-current washing is preferably practised with the water which replenishes the bath, and while in such practice the temperature regulation of the saturatoris such as to require an amount of inflowing water suflicient to thoroughly cleanse the sulfate, the invention is not restricted thereto.

I claim:

.1. In the production of sulfate of ammonia by treating coal gas in an acid saturation bath, the method herein described of freeing the sulfate of acid, consisting in sub- Plow-like arms jecting the sulfate to a cleansing liquid, with sisting in introducing coal gas into an acid saturation bath in condition to cause it to absorb water from the bath, replenishing the water content of the bath, and'"simultaneously withdrawing the ammonium sulfate in opposite direction to the entering'water and in contact therewith.

a. In the production of sulfate of am monia, the method herein described, consisting in introducing coal gas into an acid saturation bath in condition to cause it to absorb water from the bath, elevating and thereby withdrawing the ammonium sulfate from the bath, and replenishing the water content of the bath by introducing water thereinto in contra-current to the discharging sulfate and in contact therewith.

5. In apparatus for producing sulfate of ammonia, a saturator containing an acid bath adapted to receive coal gas and form ammonium sulfate, means for withdrawing the sulfate, and-means for washing the sulfate as itis being withdrawn.

6. In apparatus for producing sulfate of ammonia, a saturator containing an acid J bath adapted to receive coal gas and form ammonium sulfate, and a source of water for replenishing the bath with the water moving oppositely to and in contact with the sulfate as the latter is withdrawn.

I 7. In apparatus for producing sulfate of ammonia, a saturator containing an acid bath adapted to receive coal gas and form ammonium sulfate, a conveyer for removing the sulfate from the bath, and means for bodily shifting the conveyer relatively to the accumulation of sulfate within the saturator for causing the conveyer to act on different portions of such accumulation.

8. In apparatus for producing sulfate of ammonia, a saturator containing an acid bath adapted to receive coal gas and form ammonium sulfate, an endless vertically movable conveyer extending upwardly from the lower portion of the saturator, a con "eyer support, and means'for moving the supportabout avertical axis.

9. 1n apparatus for producing sulfate of ammonia, a saturator containing an acid bath adapted to receive coal gas and form ammonium sulfate, a support extending upently of its sulfate elevating movement, and

means for driving the' conveyer and for s1-- multaneously moving it bodily.

11. In apparatus'for producing sulfate of ammonia, a saturator containing an acid bath adapted to receive coalgas and form ammonium sulfate, a tube extending upwardly through the saturator and open to the lower portion of the latter, the upper portion of the tube open at the exterior of the saturator for discharging sulfate, and a conveyer operative within the tube for withdrawing sulfate from the saturator.

12. In apparatus for producing sulfate of ammonia, a saturator containing an acid.

bath adapted to receive coal gasand forfn ammonium sulfate, a tube extending upwardly through the saturator and open to :the lower portion of the latter, the upper portion of the tube open at the exterior of the saturator for discharging sulfate, a conveyer support rotatable in the tube about a vertical axis, and a conveyer mounted on the support.

13. In apparatus for producing sulfate of ammonia, a saturator containing anacidbath adapted to receive coalgas and form sulfate of ammonium,"a sulfate removing conveyer for withdrawing the sulfate from the bath, and a source of water, for replenishing the bath with such Water flowing through the conveyer in contra-current to the discharging sulfate.

In testimony whereof, I allix my signature in presence'of two witnesses.

HENRY a. onarnurnaf Witnesses:

LEWIS VINoEN'r, ADA M. STEELE.