DECEMBER, 1937
INDUSTRIAL AND ENGINEERING CHEMISTRY
The ingredients of the waste are mainly sodium carbonate, alkali metal soaps, and emulsified mineral oil. Such an emulsion would be decomposed by conversion of the soap to a n insoluble form. Experimental work indicated that addition of calcium chloride will convert the soap to insoluble calcium soaps which will entrain all of the emulsified oil to give it a clear and colorless effluent. I n laboratory experiments 2 and 4 cc. of 12 per cent calcium chloride solution per 100 cc. of boil-off gave the finished effluents shown in Table I. These factor weights correspond to treatment with 2 and 4 pounds of calcium chloride per 100 gallons, respectively, the calcium chloride being the commercial 75 per cent grade. For practical use a solution of calcium chloride containing about 3 pounds to the gallon would be suitable.
T+4BLE
I. RESCLTSO F TRADE WASTE TREATMENT (IN
Treatment
PARTS
~~0,000)
PER
Raw Liquor
nH
%tal solids a t 110’ C. Inorganic solids (by loss on ignition) Organic solids (by difference) Oz-consumed (permanganate method)
fi -i n _.,_
668 308 360
376
2 Lb. CaCh per 100 Gal. 7 . . 6_
394 333 61 U
4 Lb. Filtered CaC12 through per Bed of 100 Gal. Ashes 7 2 7 0 739 i4i 509 216 130 25 a
66
Not significant because chlorides are present.
The amount of calcium chloride required is substantial because the sodium carbonate must be converted to sodium chloride and calcium carbonate as well as the alkali soaps to calcium soaps. The p H of the finished effluents indicates that the reaction takes place smoothly since they are nearly neutral. Laboratory results such as these are only an indication, and for practical results it is highly probable that further reduction could be made. The process was tried out on a plant scale and operated satisfactorily with a pilot plant. The development of a simpler process rendered its complete installation unnecessary. The removal of such sludge in a relatively concentrated condition is satisfactorily carried out by filtration on a light cotton fabric. The rate of filtration is about 1 gallon per 90 square inches of filtering area per minute so that commercially about 1.25 square feet of filter area would be required per 1000 gallons per day. The sludge is curdy in nature. If it stands for several hours, it becomes oily. It was expected that the sludge would need to be filtered before it became oily but experience shows that such was not the case. A tank of calcium chloride solution was expected to feed the solution to the waste to be treated while passing through a suitable calender for mixing. As indicated by the analyses of Table I, the finished effluent is clear and transparent and harmless to fish and vegetable life. Pilot plant operation indicated a cost for materials of 20 cents per 1000 gallons. The indicated labor cost is low. The use of ashes as a filter bed was developed with the cooperation of the State of Illinois Sanitary Water Board and proved to be simpler and less expensive. The effluent was found acceptable, and analysis of a representative sample is included in Table I. The results reported with addition of calcium chloride cannot be directly compared because of the increase in solids due to the salts resulting from treatment. The effluent from the ashes contains considerable suspended matter a t times but is much clarified from the original condition. The ashes can be expected to contain substantial amounts of soluble heavy metal compounds, mainly lime. Probably the reaction of these with the soaD is similar to the reaction of calcium chloride. Since the stabilizing agent is de-
1439
stroyed by this treatment, the emulsion is broken and precipitation of the oil results. I n practice the bed used is 3 feet deep and contains 1440 cubic feet or 30 tons of ashes. It is roughly divided into three sections, and the oldest section is replaced each week. The used ashes are hauled away by local people because their oily condition makes them excellent material for building secondary roads. Each charge of 30 tons of ashes treats about 1,000,000 gallons of boil-off. It is estimated that this volume of boil-off contains 6500 pounds of oils and 1500 pounds of soap, soda ash, etc. Although this treatment has been in use for only about a year, satisfactory results have been obtained.
Acknowledgment This paper is published by permission of the Weil-Kalter Company of St. Louis, Mo., and Sparta, Ill. The cooperation of Paul Weil and A. S. Barnard is acknowledged particularly.
Literature Cited (1) Geyer, J. C., and Perry, W. A., “Textile Waste Treatment and Recovery,” p. 93, Textile Foundation, Inc., 1936. (2) Turpin, U. F., Eng. hrews-Record, 109, No. 26, 7-8 (1932). RECEIVEIDSeptember 11, 1937. Presented before the Division of Water, Sewage, and Sanitation Chemistry a t the 94th Meeting of the American Chemical Society, Rochester, N. Y., September 6 to 10, 1937.
Life of Shellacs after Heating ARTHUR A. VERNON AND ROLAND E. GILL Rhode Island State College, Kingston, R. I.
T
ESTS were made to determine how long various samples of shellac would stand heating without losing their tackiness. The samples were aged in an electric oven for varying periods and tested on an electric hot plate maintained a t 275” F. The table gives the time in seconds, after the shellac had melted, necessary for the samples to lose all tackiness when tested with a spatula. The specifications are given in the A. 8.T. M. Standards (Designations D237-33 and D207-55) :
A.
C. D. A.
B.
C. D.
After Heating a t 140’ F. Time of Heating----Shellac 0 1 hr. 2 hr. 3 hr. Refined dry bleached 0 0 0 0 Regular dry bleached 94 50 0 0
36 Regular dry bleached 137 Refined dry bleached 570 462 Grade A, orange shellac 1415 1395 After Heating a t 180’ F. Refined dry bleached 0 0 Regular dry bleached 94 0 Refined dry bleached 183 0 512 290 Grade A, orange shellac 1636 891 1153 708 866 470 Regular dry bleached 137 0 570 206 Refined dry bleached 984 Grade A, orange shellac 1415
4 hr. 0 0
30 394 1365
0 366 1137
0 17 1047
0 0 0 217 836 633 365 0 174 930
0 0 0 0 122 0 90
0 0 0 0 0 0 0
0 0
0 0
0
0
Each group represents a product of a different manufacturer. The samples were furnished through the courtesy of George Lawson. RECEIVED J ~ 23,I 1937. ~
