US2381368A - Soap preparation - Google Patents

Description

Aug. 7, 1945. J. Ross soAP PREPARATION Filed Aug. l5, 1942 i 9 l l 0 l 0 a u l D n l I 0 O O O O O O O Q O O O O O ITmJ O C O O o O 0 O O 0 G O O G .v0 #000 Ilollllbl ITM. ,Q m. n. .N .H

Ilm.

. INVENTOR. 'L/OHA/ @0.55.

ATTORNEY Patented ug. 7, 1945 SOAP PREPARATION John Boss, Ramsey, N.. J., assignor toColgate- Palmolive-Peet Company, Jersey City, N. J., a

corporation of Delaware Application August 15, 1942, Serial No. 454,909

Claims.

The present invention relates to a method for converting molten anhydrous soap to a readily usable form and, more particularly, to a process for cooling and partially hydrating molten. anhydrous soap, to an apparatus therefor, and to the product of said process.

- Anhydrous soap has been made by various ing the molten soap into and beneath the surface of a pool of water or soap 4solution and intimately mixing the soap therewith, but this method provides a soap containing a, large amount of water, part of which mustfrequently be'removed, as when it is desired to make a milled soap. The removal of the water is a costly and time-consuming operation and requires equipmentwhich occupies considerable space, all of which-are disadvantageous. It has also been suggested to cool the soap out of contact with air by carrying it through a pipe by means of a worm conveyor, the solid anhydrous soap coming out as chips at the outlet end of the pipe. This method has the disadvantage that the solid anhydrous soap is extremely'diillcult to work and/or to dissolve, so that the soap is notin a. readily usable form.

, Thus, although these and other suggestions and proposals have been made, no satisfactory method, so far as is known, has been provided for rapidly cooling molten anhydrous soap and converting it into a readily usable form.

It is an object of the present invention to provide a novel method for directly and rapidly cooling molten anhydrous soap out of contact with air without substantial change of shape and with or without partially hydrating the soap.

l of eaclrstring is partially hydrated. The strings' A It is another object of the invention to provide Other objects and advantages of this inventionwill be apparent from the following description,

taken in conjunction with the accompanying drawing, wherein:

Fig. 1 shows a longitudinal sectional view, partly diagrammatic, of an apparatus in accordance with the present invention; I I

Fig. 2 is-a fragmentary detail section taken' substantially on the line 2-2 of Fig. 1; and

Fig. 3 depicts a transverse section taken onthe .line 3--3 of Fig. 2. L

According. to this invention, molten anhydrous soap is expressed in the form of threads or strings out of contact with air .into a pool of cooling liquid. The molten soap is ecooled by contact with the liquid, and, when an aqueous body is employed as the cooling liquid, the outer portion are kept out of contact with each other for a short period Iof time, during which cooling is' continued, and the illiform soap is then removed from the pool at a temperature where oxidation upon contact with air is substantially negligible and in a condition in which the soap can be passed directly to mills and plodders for further processing. l The molten anhydrous soap may be made by .any of the methods known to the art. Thus,

fats and fatty oils and/or free fatty acids and/or esters thereof may be mixed with alkaline agents in batch, intermittent or continuous operation, and the resulting reaction mixture heated to somewhat elevated temperatures and then iiashed into a lower pressure zone to volatilize Water or other solvents, glycerine (if any), alcohols (if any), and unsaponiable matter and to recover the resulting anhydrous soap. In another method, the fatty material and alkaline agent are heated together in the absence of air and liquid water to a temperature above the melting point of the resulting anhydroussoap while passing a current of steam therethrough to remove glycerine, if any, and unsaponiiable matter. The alkaline or saponifying agents which may be used for saponifying these fatty materials include sodium and potassium hydroxides, carbonates, silicates, etc., lime, magnesium carbonate, pyridine,v

methyl morpholine, alkyl amines, alkanolamines, and other organic and inorganic bases and al'- kaline materials, and mixtures of these; 'I'he alkaline agent may be introduced in aqueous solution, in 'alcoholic solution, or in solutions of other solvents, or may be substantially anhydrous and/or substantially undiluted. It will be understood from the foregoing that molten anhy drous soap made by any other. method would be equally applicable for treatment by the present in the soap so that it is sun fluid enough to be extruded through the orifices withoutclogging them.

The pool into which the molten anhydrous soap is expressed or extruded may be of water or other suitable liquid or may be an aqueous solution of soap, sodium chloride, sodium sulphate, sodium carbonate and/or other material capable of decreasing the solubility of the soap in the water. A non-solvent for soap, such as an alkanel cycloalkane, ether or halogenated alkane or ether, may similarly be employed as the cooling liquid. The orifices may be of any desired size and shape and may be uniform or not, as desired. In general,

round orifices of about JAG inch to about 1/2 inch or larger are preferred, and 1/4 inch orifices have been found to give satisfactory results. The orifices are preferably spaced apart by a distance of about twice to about ten times their own diameters to keep the strings of soap out of contact with each other for a short time.

Another method of keeping the strings apart is to surround each oricewitha short tube larger in diameter than the orifice and open at one end to the solution in the cooling vessel.

in individual strings for as long a time as is desired before allowing them to come into contact with each other, and such length will necessarily depend upon such factors as the temperatures of the soap and of the cooling liquidand the speed at which the soap is extruded, as will be apparent to those skilled in the art.

Since the Adifference in temperature between the molten anhydrous soap and the cooling liquid is necessarily great, the temperature difference normally being over 200 C., itis preferred to provide means for keeping the cooling liquid in motion. Such means may comprise stirrers and agitators in the`cooling liquid, or, where practicable, it is preferred to flow the cooling uid across the path of travel of the soap strings. Where tubes surrounding the orifices are employed, the tubes may be perforated to permit fresh cooling liquid to come into contact with the hot soap. This has the further advantage of sweeping away the vapor which is usually formed upon contact of the soap with the cooling fluid.

The processof the invention will now be described in connection withl a novel apparatus for carrying the same into practice. Referring to the figures, reference character I designates a molten anhydrous soap supply vessel, the outlet of which is connected by means of a conduit with the inlet The length of these tubes may be adjusted to keep the soap` 9A of diameter larger than the orices 8 in the wall are perpendicularly afiixed to the inner surface of said wall 6, the end of each tube surrounding one of the orifices, and each tube has a plurality of perforations l0. The other end of each tube is open in the cooling vessel 1. A continuous mesh conveyor Il is provided in the vessel, said conveyor being at least as wide as the bank of tubes and being mounted in a position vabove said tubes and adapted to move material along the bottom of said conveyor in the same longitudinal direction as from the closed to the open ends of said tubes. A belt conveyor l2 of approximately the same width as the conveyor Il and extending in substantially the same direction is mounted with its lower end beneath the forward end of the conveyor Il' and with its upper end outside the cooling vessel and said conveyor 'l 2 is adapted to carry material upon the upper surface thereof. Means (not shown in the figures) areprovided for driving the conveyors. A liquid inlet l 3 is provided at the bottom i4 of the Vessel 'l near a side thereof perpendicular to wall 6, and a pump is adapted to y deliver cooling liquid to this inlet at a desired rate. An yoverflow outlet at the opposite side of the cooling vessel is provided for removal of the heated liquid. The overflow may be cooled, adjusted to proper composition with make-up water, solution, etc., and recirculated through the pump, if desired.

The operation of the dvice is relatively simple and will now be described in connection with the use of an aqueous body as thecooling liquid therein. Molten anhydrous soap is removed from the supply vessel l by the pump 2 and delivered to the heat exchange unit 4, where part of the heat in the soap is removed. Sufficient heat remains so that the soap'in molten, semi-molten, plastic or semi-plastic form can be forced under pressure into the manifold 5 and through the orifices 8 in the wall 6 of the cooling vessel 1. The soap is expressed through the orifices 8 into the tubes 9. At the start of the operation, since the tubes are open at one end thereof to the aqueous cooling liquid in the vessel, the tubes are filled with the cooling liquid. When the hot anhydrous soap comes into contact with the aqueous liquid in the tubes, steam is formed, and an envelope of steam attaches itself to the strings of soap. The steam tends to make the soap rise in the cooling liquid, especially where a heavy` brine of a pump 2 driven .by a motor 3. The outlet of the pump connects by means of a conduit with .a

heat exchange unit 4, and a pipe from this unit leads to a` manifold or header 5 attached to thelower portion of the outside of a wall 6 of a cooling vessel 1. The wall 6 is perforated at its lower portion with a plurality ofA orifices 8, all of which are within the area covered by the mainfold 5 upon the outside Vof the Wall. A pluraiity of tubes `tions at the lower sides.

solution is employed, and the strings of soap of anhydrous soap within thel string; Where the factors which influence the rate ofy cooling, as will be discussed infra, are such that the strings of soap are sufficiently cooled so that they will not conglomerate upon coming together, the strings -emerge from the open end of the tubes 9 and are individually carried up by the steam envelope around them to the under-surface of the'conveyor Il. They are carried along bythe conveyor until the steam which surrounds them has escaped through the mesh of the conveyor into the 4 upper portion of the cooling vessel, and the f strings then fall uponthe upper side of the conbefore flashing or heating or by simultaneously veyor I2. This second conveyor removes them from'the vessel.

The number, size and spacing of the orifices in. y

the wall of the'cooling vessel, the length ofthe tubes provided, the speed at which the strings of soap move through the liquid. as well as the rate at which the cooling liquid is circulated through the vessel, the temperature of the cooling liquid, the amount of prec'ooling of the hot anhydrous soap before extrusion through the 'oriiices, the total length of time that the soap stays in the cooling vessel, etc., are among the liform soap may be fed directlyto mills and plodders, there to have adjuvant materials incorporated therewith. Where the various factors are so adjusted that soap will conglomerate upon coming together to form a partially hydrated mass of soap, the amount of hydration can also be controlled to provide a soap which can be directly milled and plodded.

When it isdesired to produce a substantially anhydrous product, a non-aqueous cooling liquid, preferably a high-boiling organic liquid in which the soap is substantially insoluble, may be employed, as aforesaid. The soap, after cooling, may be blown to volatilize the film of liquid thereon, especially if the liquid employed is relatively low-boiling, or such film may be removed by extraction with a low-boiling solvent for the liquid, which solvent may be removed from 'the soap in turn by blowing, slight heating or like methods. Thus, white oil, kerosene, decalin and/or tetralin may be used as the cooling liquid, and the residual film upon the iliform soap may be extracted with ethyl ether, petroleum ether and/or other volatile solvent.

Adjuvant materials which may be mixed with' the soap include fatty acid soaps prepared by the same or other methods, resin acid soaps, naphthenic and alkylated naphthenic acid soaps, sulphated and suiplionated organic compounds, alkaline soap builders, water-soluble, water-softening acid compounds of phosphorus, and other salts including sodium carbonate, sodium siliflashing a second solution containing such adjuvant materials.

The present process has the advantage vof cooling anhydrous soap out of contact with air so that decomposition and discoloration of the product are avoided, while simultaneously hydrating the soap to a desiredamount suitable for processing without having to remove part ofthe Water. A further advantage of the process ist'o provide soap in a convenient and'easily handled form which may be ,easily dissolved or which may be used directly' in mills and plodders `in the manufacture of a milled soap.

It will be understood that the term molten as applied herein to the anhydrous soap treated is also intended to include said vsoap in s'emi-v molten, plastic, and semi-plastic forms.

Although the present invention has been described in connection With a. particular embodiment, it will be understood by those skilled'v in the art that other variations and modifications of the invention can be made and that various equivalents can be substituted therefor without departing from the yprinciples disclosed herein. Thus, instead of introducing the molten soap at the side of the pool of cooling l-iquid,` the orinces may be positioned at either the top or the bottqm of the pool, depending upon the gravity and boilingpoint of the liquidrused and whether the strtngs of soap will at first tend to fall or to rise upon being extruded into the cooling liquid.

cates, trisodium phosphate, borax, sodium tetraphosphate, sodium bicarbonate, sodium sulphate, sodium chloride, sodium acetate, sodium hypochlorite, sodium thiosulphate, sodium perborate,

, sodium tartrate, sodium citrate and sodium oxalate, and the corresponding-ammonium, substituted ammonium and potassium salts of the corresponding acids; insecticidal, germicidal, styptic and medicinal agents, including aluminum chloride, mercurio chloride and various copper and K lead salts; coloring agents, abrasives, llers, and

water-dispersible gums, including dyes, lakes,

pigments, silica,` kieselguhr, silica gel, feldspar,

precipitated chalk, pumice, infusorial earth, bentonite, talc, starch, Irish moss, sugar, methyl cellulose, agar, gum tragacanth, gum arabic, and polyvinyl alcohol; liquids, such as ethyl alcohol, glycerol, cyclohexanol, naphtha, benzene, kerosene, turpentinefpine oil, decalin and tetralin and `I the like. The type of addition-agent will depend upon the ultimate use of the new composition. Other ways of incorporating these addition agents besides mixing the final' product therewith are to admix the adjuvant materials with the raw fatty material and/or the saponifying agents Such arrangement may sufiice in some cases to keep the strings separated from each otherfuntil cool. It will also be appreciated that, although the extruded soap has been described as in filamentous form, the orifices may be of .such shape and dimensions that ribbons, sheets, and the like can be produced. 'Ihese and other variations and modicationsare believed to be within the scope of the present specification and within the purview of the appended claims.

I claim:

1. A process of treating molten anhydrous soap which comprises extruding molten anhydrous soap through a plurality of orifices into a body o f an aqueous cooling liquid, maintaining the strings of soap so formed out of contact with each other for ,a time intervalv sulcient for cooling said strings below the temperatures of substantial conglomeration and of substantial oxidation in the presence of air and insuiiicient for substantially changingv the shape of the. soap and for more than partially hydrating said soap, and resoap out of contact with an oxidizing medium through a plurality of oriicesinto and below the surface of a body of an aqueous cooling liquid, maintaining said soap extrusions therein out of contact with eachother until partially hydrated and cooled below the temperature of substantial conglomeration, andremovingv said partially hydrated soap fromsaid liquid ,body without substantial change in shape.

3. A process of treating molten anhydrous soap which comprises passing continuous strings of molten anhydrous soap through a body of an aqueous cooling liquid, maintaining said strings therein out of contact witheach other until partially hydrated and cooled below the temperature vof vsubstantial conglomeration, continuously removing said partially hydrated soap in filamen- 4 f a i 2,381,368

tous form from said liquid body, and milling and plodding said filiform soap.

4. A process of treating molten anhydrous soap which comprises extruding molten anhydrous soap out of contact with an oxidizing'medium through a plurality of orices into and below the surface of a body of a high-boiling organic liquid wherein the soap is substantially insoluble, maintaining saidsoap extrusions therein out of contact with each other until cooled below the temperature of substantial conglomeration, removing said soap from said organic liquid body without substantial change in shape, washing said soap with a volatile-organic solvent wherein residual high-boiling organic liquid upon said soap is soluble and wherein the soap is substantially insoluble, and vaporizing residual volatile solvent from said soap. A

5. A process of treating moltenanhydrous soap which comprises extruding the molten anhydrous soap through a .plurality of orifices into a body of a cooling liquid, maintaining the strings of soap so formed out of contact with each other for a time sulcient for cooling said strings below the temperature of substantial conglomeration, andJ removing said cooled soap from said body of liquid.

JOHN ROSS.

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