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US3152947A - Process for drying higher fatty acid sarcosines - Google Patents

Process for drying higher fatty acid sarcosines Download PDF

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US3152947A
US3152947A US225408A US22540862A US3152947A US 3152947 A US3152947 A US 3152947A US 225408 A US225408 A US 225408A US 22540862 A US22540862 A US 22540862A US 3152947 A US3152947 A US 3152947A
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sarcosinate
fatty acid
solution
higher fatty
sarcosines
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US225408A
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Monick John Alexander
Lehmacher William Hubert
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Colgate Palmolive Co
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Colgate Palmolive Co
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00Drying solid materials or objects by processes involving the application of heat

Definitions

  • the present invention relates to a process for heat drying aqueous solutions of higher fatty acid sarcosines and salts thereof.
  • Higher fatty acid sarcosines are useful as constituents I of dental preparations such as tooth pastes and powders,
  • the higher fatty acid sarcosine be available in dry solid form, preferably a particulate solid form.
  • the fatty acid sarcosines and their salts are more stable toward chemical and biological decomposition when in dry solid form than when in the form of an aqueous solution..
  • a drying step is necessitated.
  • the drying of such solutions presents a troublesome problem.
  • sarcosines are difficult to dry satisfactorily by conventional methods because of their tendency to decompose on exposure to elevated temperatures for an extended period of time.
  • sarcosines are also characterized by a tendency to gel when in high concentrations in aqueous solutions. Such gels are characterized by very poor heat and mass transfer rates, and are very difficult to dry without experiencing thermal decomposition of the sarcosine.
  • the normally solid sarcosines contemplated as within the present invention are amides formed from sarcosine and a higher fatty acid or mixtures thereof. These fatty acids are straight chain higher mono-carboxylic acids containing from to 18 carbon atoms and may be saturated or unsaturated as long as the sarcosine derivative or salt thereof is normally solid. Examples of such fatty acids are lauric acid, myristic acid, palmitic acid, oleic acid,
  • a process for heat drying aqueous higher fatty acid sarcosines and their salts has now been discovered which is characterized by advantages of reduced thermal decomposition during processing, substantially "quantitative recovery of fatty acid sarcos-ine solids (c.g. greater than 99%) and the production of dust-free dry products.
  • coconut oil fatty acids and hydrogenated. tallow fatty acids, it being especially preferred to carry out the present process employing those fatty acid sarcosines which either because of their relatively low stability, low melting point or tendency to gel, or combination of such characteristics, cannot be dried in conventional ways into discrete, non-dusty particles.
  • fatty acid sarcosines which readily form gels when in high concentration in aqueous solution are those higher fatty acid sarcosines prepared from straight chain saturated fatty acids containing 12 to 16 carbon atoms, and especially the sodium salts thereof.
  • the sarcosines of the present invention may be in the acid form or may be employed as a salt (sarcosinate) and the term higher fatty acid sarcosine as used herein and in the appended claims is intended to encompass Within its scope both the acid' and its salts. It is preferred to employ salts selected from those formed by alkali metals or nitrogen-containing radicals. More particularly they may be sodium, potassium, ammonium, amine, niono-, di, or tri-ethanolamine salts. It is particularly preferred to carry out the present process employing the sodium salts of sarcosinates whose fatty'acyl groups are saturated and contain from 12 to 16 carbon atoms.
  • the presenthigher fatty acid sarcosines may be made by condensing a fatty acid chloride'or a mixture of fatty acid chlorides with sarcosine in thepresence of a hydrogen halide acceptor, e.g. caustic soda, soda ash, magnesium hydroxide, trimethyl amine.
  • a hydrogen halide acceptor e.g. caustic soda, soda ash, magnesium hydroxide, trimethyl amine.
  • the resulting amide is separated, acid washed and subsequently, if desired, neutralized with a .base containing a desired cation.
  • a gelation concentration is the upper feasible solution concentration limit of the aqueous solutions dried in carrying out the present process.
  • solvents such as ethanol and isopropanolis within the scope of the present invention as these solvents are removed along with Negligible increase in free fatty acid content is experienced in the course .of drying higher fatty acid sarcosines in accordance with the present procedure, thus facilitatingpreparation of higher fatty acid sarcosiues containing less than- 15% free fatty acid, (or fatty acid 1 soap) which is preferred for use in dentifrices.
  • solvents such as ethanol and isopropanolis within the scope of the present invention as these solvents are removed along with Negligible increase in free fatty acid content is experienced in the course .of drying higher fatty acid sarcosines in accordance with the present procedure, thus facilitatingpreparation of higher fatty acid sarcosiues containing less than- 15% free fatty acid, (or fatty acid 1 soap) which is preferred for use in dentifrices.
  • a continuous V processfor heat drying a higher fatty acid sarcosine comprises forming a thinlayer of a fluid aqueous solution of a higher'fatty acid sarcosine, heating said layer to a temperature sufiicient to boil off the water therein and melt said higher fatty acid sarcosine for a time sufiicient higher fatty acid sarcosine substantially pure and containing from 10 to 48% total. solids.
  • solution is used herein to describe fluid aqueous preparations including true solutions, suspensions, collodial suspensions, dispersions, and slurries, but
  • aqueous solutions may contain other'liquid ingredients such as low molecular weight alcohols, e.g. ethanol and ,is opropanol whichserve to diminish solution viscostiy and toy increase the extent of fatty acid sarcosinate solubilty without gel formation,
  • the sarcosine should be as free as possible of fatty acids and fatty acid soaps because of the deactivating properties thereof.
  • the fluid aqueous higher fatty acid sarcosine preheated if desired but normally at a temperature below about 100 C., is disposed as a thin moving layer of liquid from which solvent is vaporized as the layer progresses through a heating zone.
  • the layer employed is preferably disposed on a heated metallic surface and is less than A inch thick, preferably being a thin film having a thickness of less than inch, typically between and of an inch.
  • the layer of higher fatty acid sarcosine is heated to a temperature which is above the boiling point of the solvent from the aqueous layer and above the melting point of the higher fatty acid sarcosine solid, typically to a temperature on the order of 145195 C., in the case of the salts, and 105145 C. in the case of the lower melting free acids.
  • the layer progresses through the heated zone it is maintained at a temperature above its boiling point for a period of time sufficient for substantially all of the solvent therein to evaporate or boil off, and to form substantially dry molten fatty acid sarcosine, but insuflicient to cause any significant pyrolytic decomposition of the higher fatty acid sarcosine.
  • a period of time of exposure to elevated temperature is on the order of less than 2 minutes, and preferably less than 30 seconds, typically being on the order to to 30 seconds.
  • the molten higher fatty acid sarcosine is then removed from the heated zone and immediately is cooled to a stable solid condition to form a rigid solid product containing less than about 6%, and preferably less than about 2% moisture as at moisture levels of about 6.5% and above, non-rigid tacky gels tend to form.
  • the thin layer of higher fatty acid sarcosine which is processed in accordance with the present invention is agitated throughout the boiling period. While suitable turbulence may be obtained by means of turbulent fluid flow, it is much preferred to carry out the instant process employing mechanical agitation of a thin film of liquid being heated on a metallic surface.
  • the dry molten fatty acid sarcosine may be cooled in any suitable manner to form flakes, pellets, ribbons, powder, granules, spheres, strips, bulk form, or the like. It is preferred to form dense, non-dusty readily soluble solid pellets of maximum diameter less than about inch by forming the molten fatty acid sarcosine into discrete liquid droplets which are solidified by spray cooling, immersion in a cool, non-solvent liquid, or deposition on a chilled surface, e.g. a cooling roll. Such dense particulate solids have a high bulk density and are economical to ship, and are readily wetted by water, dissolving easily without floating or foaming.
  • FIG. 2 is a section taken on line 22 of FIG. 1;
  • FIG. 3 is a section taken on line 33 of FIG. 1.
  • the apparatus of FIGS. 1-3 comprises a wiped film evaporator 18, a cooler 20, and a product collection bin 22.
  • the wiped film evaporator comprises essentially a closed vertically elongated tube 38 containing a concentrically mounted rapidly rotating vaned agitator 40 which forces the liquid content of the evaporator against the inner wall of said vertical elongated tube 38 thus spreading the liquid in a thin film and maintaining the liquid in rapid movement so as to insure intimate mixing, heat transfer and prevent overheating.
  • a feed supply nozzle 36 is located in the upper portion of the tube 38.
  • the portion of the vertical tube 38 below the feed point 36 of the evaporator 18 is provided with a jacket 39 through which a heating medium is passed, the heating medium entering and leaving said jacket by means of taps 44 and 46 at the base and top thereof respectively.
  • the liquid content of the evaporator flows down the inside surface of the tube $8, through a spider 48 which carries a foot bearing 49 supporting the vaned agitator 4t ⁇ , and collects in a closed cylindrical distributor 50 which is provided with perforations 51 near the outer edge of the base thereof.
  • the distributor is steam traced (not shown) in order to, prevent cooling and solidification of the material therein.
  • Liquids passing through the perforations fall as droplets on a rotating drum 52 which is chilled by cooling water supplied to the interior thereof through hollow trunnions 54 and 56. Material is removed from the surface of the cooling roll by a doctor blade 58, and falls into the product collection bin 22.
  • the portion of the vertical elongated tube 38 above the feed point 36 forms a separation chamber 60 for recovery of liquid entrained in the vapors being removed.
  • a conduit 62 which communicates with the separation cham ber 69, is connected to a source of slight vacuum (on the order of 4 millimeters of water) so as to facilitate removal of solvent vapors from the reactor 18.
  • the vaned agitator 40 is rotated by a belt 64 driven byan electric motor 66.
  • a 36% fluid aqueous solution of (99% sodium N-lauroyl sarcosinate and 1% lauric acid soap) solids is fed at room temperature of 25 C. to the evaporator through the feed conduit 36-at a rate of pounds of solution per hour for a 4-hour period. Rapid rotation of the agitator spreads and turbulently agitates the solution as a thin film on the interior of wall 38 of the evaporator, the clearance between the periphery of the vanes 40 and wall 38 and the thickness of the film being approximately A2 inch.
  • Saturated steam at p.s.i.g. (C.) is supplied to the jacket through tap 46, and condensate is removed at tap 44.
  • Vapors at a temperature of 102 C. v are removed through conduit 62 by application thereto of a vacuum of 4 millimeters of water.
  • the vaporizing surface in the evaporator is 9 square feet, and the agitator runs at 900 r.p.rn., corresponding to a peripheral velocity of 2,820
  • substantially dry sodium N-lauroyl sarcosinate issues from the base of the evaporator and falls into the distributor head 50 from which it issues as droplets through the holes 51 and falls onto the cooling roll 52, the time of passage from the feed conduit to the cooling roll being approximately 22 seconds.
  • the holes inthe distributor. are made by a No. 30 drill, and the pellets which form on the cooling roll are flattened droplets approximately A inch thick and of an inch in diameter. The pellets are removed from the cooling roll at approximately 25 C. by the. doctor blade'58 and fall into the collection bin 22.
  • the product contains 97.6% sodium N-lauroyl sarcosinate, 1.0%1auric acid soap, and
  • Example II The procedure of Example I is repeated employing a fluid feed solution containing 39.6% sodium N-lauroyl sarcosinate, 0.4% sodium laurate, 40% Water, and 20% ethanol at room temperature.
  • the feed rate is 30 pounds per hour per square foot of heated surface in the evaporator, and the evaporator is heated with saturated steam at 'about 145 C. No increase in soap content is experienced, the product being solid, free-flowing, non-tacky, rigid, alcohol-free particles which contain 93.25% sodium N-lauroyl sarcosinate, 5.75% moisture, and 1.0%
  • Example 111 The procedure of Example II is repeated employing, as a feedstock, a fluid mixture containing 85% molten N- lauroyl sarcosine (melting point about 45 C.) and 15% water.
  • the feed rate is 2.0 pounds per hour per square foot of heated surface, and the temperature of the teed is about 75 C.
  • the saturated steam used is at about 127 C.
  • the product obtained contains 98.2% N- lauroyl sarcosine, 1.5 free fatty acid, and 0.3% moisture.
  • FIG. 4 shows diagrammatically the various components of an alternate apparatus for carrying out the process of the present invention. It comprises a commercially available thin film heater '70 constructed in a manner similar-to a conventional plate and frame filter 'press that it consists of a plurality of thin corrugated rectangular sheets 72 clamped between two end plates 74, '76 (by means not shown), a centrifugal liquid-vapor I separator 77, a liquid distributor 7 8, a product cooler 79,
  • FIG. 5 illustrates a typical construction of one of the sheets '72.”
  • the sheets are spaced and sealedby gaskets 81 around their outer edges and are provided, in a manner similar to the plates of a conventional plate and frame filter press, with openingsiZ, S3, 84 and 85 in each corner for flow of fluid. These openings may be communicated with or sealed off from the space between any pair [of adjacent plates by virtue of the shape of the gaskets blemployed.
  • openings tvit and d5 communicate with the illustratedsurfaceof the plate 72,-and openings 82 and 84 head dispense droplets onto the cooler 79.
  • the plate to plate spacing throughwhich the fluid flows averages from $4 to of an inch, thus providing, in the space between each pair of plates, for the formation of a turbulently flowing stream consisting, in essence, of two liquid layers each from A to of an inch thick.
  • the heater of FIG. 4 is provided with a conduit 88 through which heating medium is supplied to the plates and a conduit 89 for exhausting the used heating medium.
  • a conduit 90 supplies feed to be heated to the spaces between the plates, and a conduit 92 is provided for removal of the heated product.
  • the product conduit 92 is tangentially connected into the periphery of a centrifugal separator 77 comprising a closed cylindrical vessel 94; provided with an overhead line 98 for removal of vapors and a drain conduit 100 for removal of liquids.
  • a center post 102 is provided to maintm'n regular circulation of materials in the separator and to prevent turbulence.
  • the drain conduit 100 supplies the distribution head 78. Perforations 101 in the bottom of the distribution In use, the separator 77, the drain conduit 100, and the distribution head 78 are steam traced (not shown) to insure that the materials therein are maintained in molten condition.
  • the cooler 79 comprises a cooling roll 104 which is chilled by means of cold water supplied-thereto through hollow trunnions 106 and 108. Cooled material is removed trom the surface of the cooling roll by a doctor blade 119 and falls into the collection bin 80.
  • a 38% aqueous solution of 98.5% sodium 'N-lauroyl sarcosinate and 1.5% sodium laurate is fed to as a heating medium and is passed through the space between alternate pairs of plates.
  • the solution boils in the heater and forms a mixture of steam and molten so dium N-lauroyl sarcosinate which issues from the heater through conduit 92 and passes into the centrifugal separator 77.
  • Water vapors are removed from the separator through the overhead line 98 by the application thereto of a vacuum of 4 millimeters of water, and liquid sodium N-lauroyl sarcosinate drains from the base of the separator through the drain conduit 190 into the distributor 78.
  • the pellets produced contain 95% sodium N-lauroyl sarcosinate, 2.5% lauric acid soap, and 2.5% moisture.
  • a continuous process for heat drying of fluid aque ous solution of a normally rigid solid higher fatty acid sarcosinate which comprises moving such solution turbulently over a heated metallic surface in direct contact therewith, heating said solution thereby to a temperature above both the boiling point of the solution and the melting point of the sarcosinate, vaporizing substantially all of the aqueous solvent from said solution and melting the substantially dry sarcosinate thus formed before contact with any substantial amount of gas other than said vapor, forming the molten dried sarcosinate into discrete liquiddroplets, and cooling said droplets to rigid solid pellets of dry sarcosinate.
  • a continuous process for converting an aqueous solution of sodium N-lauroyl sarcosinate at a solids concentration within the range of about 10% to 40% into solid pellets having a moisture content not exceeding about 6% which comprises moving a stream of said solution continuously through a passageway, agitating and.
  • an aqueous higher fatty acid sarcosinate salt which is normally a rigid solid'comprising forming a flowable non-gelled aqueous solution of a normally solid higher fatty acid sarcosinate salt havinga tendency to gel when in aqueous solution at high concentration, disposing said flowable sarcosinate solution as a'wiped liquid film, turbulently agitating and I rapidly heating said film of sarcosinate solution to a'temperature.
  • a continuous process for heat drying, with minimum decomposition, an aqueous higher fatty acid sarcosinate which is normally a rigid solid comprising forming, at a temperature below C., an aqueous solution containing from about 10 to 40% by weight of a higher fatty acid sarcosinate, said fatty acid being a straight chain monocarboxylic acid containing from 12 to- 16 carbon atoms, disposing said solution as a wiped liquid film less than inch thick on a heated metallic surface, turbulently agitating and rapidly heating said film to a temperature above the melting point of said sarcosinate for a period of from 10 to 30 seconds sufiicient to boil oif substantially all of the water therein and produce said higher fattyacid sarcosinate in molten, substantially dry fornn forrning droplets of said sarcosinate and immediately cooling said droplets to a temperature below about 40 C. to produce hi her fatty acid sarcosinate in the form of rigid, substantially dry,
  • a continuous process for heat drying an aqueous solution of a normally rigid solid higher fatty acid sarcosinate which comprises moving turbulently a wiped layer of a fluid aqueous solution thereof over a heated surface, heating said layer to a temperature above both the boiling point of said solution and the melting point of said fatty acid sarcosinate, vaporizing substantially all of the water in said layer and melting the substantially dry fatty acid sarcosinate thus formed, forming said molten fatty acid sarcosinate into discrete liquid droplets, and cooling said droplets to rigid solid pellets of dry, higher fatty acid sarcosinate.

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Description

Oct. 13, 1964 J. A. MONICK ETAL PROCESS FOR DRYING HIGHER FATTY ACID SARCOSINES Original Filed July 7, 1958 2 Sheets-Sheet 1 JNVENTORS JOH/VAZEXflNDfR MON/CK W/lU/lMl/UBLRTLEHMACHER I g ATTORNEY Oct. 13,1964 J. A. MONICK ETAL 3,152,947
PROCESS FOR DRYING HIGHER FATTY ACID SARCOSINES Original Filed July 7, 1958 2 Sheets-Sheet 2 zlvvswozzs JOH/VALfXANDER ON/CK VWZU/IMHUBERTLEHMHCHER BY MM ATTORNEY United. States Patent The present invention relates to a process for heat drying aqueous solutions of higher fatty acid sarcosines and salts thereof.
Higher fatty acid sarcosines are useful as constituents I of dental preparations such as tooth pastes and powders,
in detergent bars, and like compositions.
For a number of such uses, e.g. incorporation in tooth powders and dry detergent compositions, it is desirable that the higher fatty acid sarcosine be available in dry solid form, preferably a particulate solid form. The fatty acid sarcosines and their salts are more stable toward chemical and biological decomposition when in dry solid form than when in the form of an aqueous solution.. Also, when the product must be transported shipping costs are lower. Inasmuch as the usual manufacturing process produces the higher fatty acid sarcosines in aqueous solution, a drying step is necessitated. However, due to the peculiar properties of the-higher fatty acid sarcosines and concentrated solutions thereof, the drying of such solutions presents a troublesome problem.
Higher fatty acid sarcosines are difficult to dry satisfactorily by conventional methods because of their tendency to decompose on exposure to elevated temperatures for an extended period of time. sarcosines are also characterized by a tendency to gel when in high concentrations in aqueous solutions. Such gels are characterized by very poor heat and mass transfer rates, and are very difficult to dry without experiencing thermal decomposition of the sarcosine.
The higher fatty acid,
ice
.The normally solid sarcosines contemplated as within the present invention are amides formed from sarcosine and a higher fatty acid or mixtures thereof. These fatty acids are straight chain higher mono-carboxylic acids containing from to 18 carbon atoms and may be saturated or unsaturated as long as the sarcosine derivative or salt thereof is normally solid. Examples of such fatty acids are lauric acid, myristic acid, palmitic acid, oleic acid,
It has previously been proposed to overcome these 7 of the zone as is amixture of spent drying gas and cooling air.
A process for heat drying aqueous higher fatty acid sarcosines and their salts has now been discovered which is characterized by advantages of reduced thermal decomposition during processing, substantially "quantitative recovery of fatty acid sarcos-ine solids (c.g. greater than 99%) and the production of dust-free dry products.
coconut oil fatty acids, and hydrogenated. tallow fatty acids, it being especially preferred to carry out the present process employing those fatty acid sarcosines which either because of their relatively low stability, low melting point or tendency to gel, or combination of such characteristics, cannot be dried in conventional ways into discrete, non-dusty particles. Examples of sarcosines which readily form gels when in high concentration in aqueous solution are those higher fatty acid sarcosines prepared from straight chain saturated fatty acids containing 12 to 16 carbon atoms, and especially the sodium salts thereof.
The sarcosines of the present invention may be in the acid form or may be employed as a salt (sarcosinate) and the term higher fatty acid sarcosine as used herein and in the appended claims is intended to encompass Within its scope both the acid' and its salts. It is preferred to employ salts selected from those formed by alkali metals or nitrogen-containing radicals. More particularly they may be sodium, potassium, ammonium, amine, niono-, di, or tri-ethanolamine salts. It is particularly preferred to carry out the present process employing the sodium salts of sarcosinates whose fatty'acyl groups are saturated and contain from 12 to 16 carbon atoms.
The presenthigher fatty acid sarcosines may be made by condensing a fatty acid chloride'or a mixture of fatty acid chlorides with sarcosine in thepresence of a hydrogen halide acceptor, e.g. caustic soda, soda ash, magnesium hydroxide, trimethyl amine. The resulting amide is separated, acid washed and subsequently, if desired, neutralized with a .base containing a desired cation. Ordinarily the sarcosine or sarcosinate is obtained in solution, and to promote economical drying of such a formed at room temperature and above, such a gelation concentration is the upper feasible solution concentration limit of the aqueous solutions dried in carrying out the present process. The addition of solvents such as ethanol and isopropanolis within the scope of the present invention as these solvents are removed along with Negligible increase in free fatty acid content is experienced in the course .of drying higher fatty acid sarcosines in accordance with the present procedure, thus facilitatingpreparation of higher fatty acid sarcosiues containing less than- 15% free fatty acid, (or fatty acid 1 soap) which is preferred for use in dentifrices.
lnaccordance with the present invention a continuous V processfor heat drying a higher fatty acid sarcosine comprises forming a thinlayer of a fluid aqueous solution of a higher'fatty acid sarcosine, heating said layer to a temperature sufiicient to boil off the water therein and melt said higher fatty acid sarcosine for a time sufiicient higher fatty acid sarcosine substantially pure and containing from 10 to 48% total. solids.
The word solution is used herein to describe fluid aqueous preparations including true solutions, suspensions, collodial suspensions, dispersions, and slurries, but
is exclusive of gels. These aqueous solutions may contain other'liquid ingredientssuch as low molecular weight alcohols, e.g. ethanol and ,is opropanol whichserve to diminish solution viscostiy and toy increase the extent of fatty acid sarcosinate solubilty without gel formation,
bacteria or microorganisms.
as fillers, additives or impurities which do not significantly detract from the utility of the product or seriously interfere with the present process, however, when intended for I used in dental preparations for its acid inhibiting effect the sarcosine should be as free as possible of fatty acids and fatty acid soaps because of the deactivating properties thereof.
In carrying out the instant drying procedure, the fluid aqueous higher fatty acid sarcosine, preheated if desired but normally at a temperature below about 100 C., is disposed as a thin moving layer of liquid from which solvent is vaporized as the layer progresses through a heating zone. The layer employed is preferably disposed on a heated metallic surface and is less than A inch thick, preferably being a thin film having a thickness of less than inch, typically between and of an inch. In the previously mentioned heated zone the layer of higher fatty acid sarcosine is heated to a temperature which is above the boiling point of the solvent from the aqueous layer and above the melting point of the higher fatty acid sarcosine solid, typically to a temperature on the order of 145195 C., in the case of the salts, and 105145 C. in the case of the lower melting free acids.
As the layer progresses through the heated zone it is maintained at a temperature above its boiling point for a period of time sufficient for substantially all of the solvent therein to evaporate or boil off, and to form substantially dry molten fatty acid sarcosine, but insuflicient to cause any significant pyrolytic decomposition of the higher fatty acid sarcosine. Typically, such a period of time of exposure to elevated temperature is on the order of less than 2 minutes, and preferably less than 30 seconds, typically being on the order to to 30 seconds. The molten higher fatty acid sarcosine is then removed from the heated zone and immediately is cooled to a stable solid condition to form a rigid solid product containing less than about 6%, and preferably less than about 2% moisture as at moisture levels of about 6.5% and above, non-rigid tacky gels tend to form.
The thin layer of higher fatty acid sarcosine which is processed in accordance with the present invention is agitated throughout the boiling period. While suitable turbulence may be obtained by means of turbulent fluid flow, it is much preferred to carry out the instant process employing mechanical agitation of a thin film of liquid being heated on a metallic surface.
The dry molten fatty acid sarcosine may be cooled in any suitable manner to form flakes, pellets, ribbons, powder, granules, spheres, strips, bulk form, or the like. It is preferred to form dense, non-dusty readily soluble solid pellets of maximum diameter less than about inch by forming the molten fatty acid sarcosine into discrete liquid droplets which are solidified by spray cooling, immersion in a cool, non-solvent liquid, or deposition on a chilled surface, e.g. a cooling roll. Such dense particulate solids have a high bulk density and are economical to ship, and are readily wetted by water, dissolving easily without floating or foaming.
In order to indicate more specifically the advantages and features of the novel process of the present invention, the following examples are set forth, which taken in conjunction with the accompanying drawings, illustrate preferred form of apparatus for carrying out the present invention. In these examples all parts and percentages are by weight unless otherwise specified.
Example 1 FIG. 2 is a section taken on line 22 of FIG. 1; and
FIG. 3 is a section taken on line 33 of FIG. 1.
The apparatus of FIGS. 1-3 comprises a wiped film evaporator 18, a cooler 20, and a product collection bin 22. The wiped film evaporator comprises essentially a closed vertically elongated tube 38 containing a concentrically mounted rapidly rotating vaned agitator 40 which forces the liquid content of the evaporator against the inner wall of said vertical elongated tube 38 thus spreading the liquid in a thin film and maintaining the liquid in rapid movement so as to insure intimate mixing, heat transfer and prevent overheating. A feed supply nozzle 36 is located in the upper portion of the tube 38. The portion of the vertical tube 38 below the feed point 36 of the evaporator 18 is provided with a jacket 39 through which a heating medium is passed, the heating medium entering and leaving said jacket by means of taps 44 and 46 at the base and top thereof respectively. The liquid content of the evaporator flows down the inside surface of the tube $8, through a spider 48 which carries a foot bearing 49 supporting the vaned agitator 4t}, and collects in a closed cylindrical distributor 50 which is provided with perforations 51 near the outer edge of the base thereof. The distributor is steam traced (not shown) in order to, prevent cooling and solidification of the material therein.
Liquids passing through the perforations fall as droplets on a rotating drum 52 which is chilled by cooling water supplied to the interior thereof through hollow trunnions 54 and 56. Material is removed from the surface of the cooling roll by a doctor blade 58, and falls into the product collection bin 22.
The portion of the vertical elongated tube 38 above the feed point 36 forms a separation chamber 60 for recovery of liquid entrained in the vapors being removed. A conduit 62, which communicates with the separation cham ber 69, is connected to a source of slight vacuum (on the order of 4 millimeters of water) so as to facilitate removal of solvent vapors from the reactor 18. The vaned agitator 40 is rotated by a belt 64 driven byan electric motor 66.
In operation a 36% fluid aqueous solution of (99% sodium N-lauroyl sarcosinate and 1% lauric acid soap) solids is fed at room temperature of 25 C. to the evaporator through the feed conduit 36-at a rate of pounds of solution per hour for a 4-hour period. Rapid rotation of the agitator spreads and turbulently agitates the solution as a thin film on the interior of wall 38 of the evaporator, the clearance between the periphery of the vanes 40 and wall 38 and the thickness of the film being approximately A2 inch. Saturated steam at p.s.i.g. (C.) is supplied to the jacket through tap 46, and condensate is removed at tap 44.
Vapors at a temperature of 102 C. v are removed through conduit 62 by application thereto of a vacuum of 4 millimeters of water. The vaporizing surface in the evaporator is 9 square feet, and the agitator runs at 900 r.p.rn., corresponding to a peripheral velocity of 2,820
feet per minute at the outer edges of the vanes. Molten,
substantially dry sodium N-lauroyl sarcosinate issues from the base of the evaporator and falls into the distributor head 50 from which it issues as droplets through the holes 51 and falls onto the cooling roll 52, the time of passage from the feed conduit to the cooling roll being approximately 22 seconds. The holes inthe distributor. are made by a No. 30 drill, and the pellets which form on the cooling roll are flattened droplets approximately A inch thick and of an inch in diameter. The pellets are removed from the cooling roll at approximately 25 C. by the. doctor blade'58 and fall into the collection bin 22.
Analysis of the product obtained in the collection bin discloses that there has been no increase in the soap content during processing. The product contains 97.6% sodium N-lauroyl sarcosinate, 1.0%1auric acid soap, and
soap.
Example II The procedure of Example I is repeated employing a fluid feed solution containing 39.6% sodium N-lauroyl sarcosinate, 0.4% sodium laurate, 40% Water, and 20% ethanol at room temperature. The feed rate is 30 pounds per hour per square foot of heated surface in the evaporator, and the evaporator is heated with saturated steam at 'about 145 C. No increase in soap content is experienced, the product being solid, free-flowing, non-tacky, rigid, alcohol-free particles which contain 93.25% sodium N-lauroyl sarcosinate, 5.75% moisture, and 1.0%
Example 111 The procedure of Example II is repeated employing, as a feedstock, a fluid mixture containing 85% molten N- lauroyl sarcosine (melting point about 45 C.) and 15% water. The feed rate is 2.0 pounds per hour per square foot of heated surface, and the temperature of the teed is about 75 C. The saturated steam used is at about 127 C. The product obtained contains 98.2% N- lauroyl sarcosine, 1.5 free fatty acid, and 0.3% moisture.
Example IV Example V FIG. 4 shows diagrammatically the various components of an alternate apparatus for carrying out the process of the present invention. It comprises a commercially available thin film heater '70 constructed in a manner similar-to a conventional plate and frame filter 'press that it consists of a plurality of thin corrugated rectangular sheets 72 clamped between two end plates 74, '76 (by means not shown), a centrifugal liquid-vapor I separator 77, a liquid distributor 7 8, a product cooler 79,
and a collection bin $0. v
FIG. 5 illustrates a typical construction of one of the sheets '72." The sheets are spaced and sealedby gaskets 81 around their outer edges and are provided, in a manner similar to the plates of a conventional plate and frame filter press, with openingsiZ, S3, 84 and 85 in each corner for flow of fluid. These openings may be communicated with or sealed off from the space between any pair [of adjacent plates by virtue of the shape of the gaskets blemployed. Thus in the embodiment illustrated in FIG. 5, openings tvit and d5 communicate with the illustratedsurfaceof the plate 72,-and openings 82 and 84 head dispense droplets onto the cooler 79.
space between surfaces of adjacent plates. The plate to plate spacing throughwhich the fluid flows averages from $4 to of an inch, thus providing, in the space between each pair of plates, for the formation of a turbulently flowing stream consisting, in essence, of two liquid layers each from A to of an inch thick.
The heater of FIG. 4 is provided with a conduit 88 through which heating medium is supplied to the plates and a conduit 89 for exhausting the used heating medium. A conduit 90 supplies feed to be heated to the spaces between the plates, and a conduit 92 is provided for removal of the heated product.
The product conduit 92 is tangentially connected into the periphery of a centrifugal separator 77 comprising a closed cylindrical vessel 94; provided with an overhead line 98 for removal of vapors and a drain conduit 100 for removal of liquids. A center post 102 is provided to maintm'n regular circulation of materials in the separator and to prevent turbulence.
The drain conduit 100 supplies the distribution head 78. Perforations 101 in the bottom of the distribution In use, the separator 77, the drain conduit 100, and the distribution head 78 are steam traced (not shown) to insure that the materials therein are maintained in molten condition.
The cooler 79 comprises a cooling roll 104 which is chilled by means of cold water supplied-thereto through hollow trunnions 106 and 108. Cooled material is removed trom the surface of the cooling roll by a doctor blade 119 and falls into the collection bin 80.
In operation a 38% aqueous solution of 98.5% sodium 'N-lauroyl sarcosinate and 1.5% sodium laurate is fed to as a heating medium and is passed through the space between alternate pairs of plates. The solution boils in the heater and forms a mixture of steam and molten so dium N-lauroyl sarcosinate which issues from the heater through conduit 92 and passes into the centrifugal separator 77. Water vapors are removed from the separator through the overhead line 98 by the application thereto of a vacuum of 4 millimeters of water, and liquid sodium N-lauroyl sarcosinate drains from the base of the separator through the drain conduit 190 into the distributor 78. Droplets of sodium N-lauroyl sarcosinateissue from the distributor, fall onto the cooling roll 104where they are immediately cooled'below their solidification point and form. small solid pellets, and are removed from the roll by the doctor blade and collected in the pan 80. The total time of passage from the feed conduit 90 to the cooler 79 is on the order'ot less than 45 seconds.
The pellets produced contain 95% sodium N-lauroyl sarcosinate, 2.5% lauric acid soap, and 2.5% moisture.
The effectiveness of heating the material being dried to a temperature above its melting point, as in the foregoing examples, is illustrated by simulating the procedure of .EXarnple I using as a heating medium, saturated steam ployed. I The solution concentrates only" to about 40% solids, and themes it approaches the gel condition, be-
comes so viscous that it cannot be removed from the The advantages of the present base of the evaporator. I process which readily producesa free-flowing, substantially-dry molten product are apparent. I 3' i This applicaiton is a continuation of our pending application SN. 746,763, filedjluly 7, 1958, now abandoned.
What is claimed is:
l. A continuous process for heat drying of fluid aque ous solution of a normally rigid solid higher fatty acid sarcosinate which comprises moving such solution turbulently over a heated metallic surface in direct contact therewith, heating said solution thereby to a temperature above both the boiling point of the solution and the melting point of the sarcosinate, vaporizing substantially all of the aqueous solvent from said solution and melting the substantially dry sarcosinate thus formed before contact with any substantial amount of gas other than said vapor, forming the molten dried sarcosinate into discrete liquiddroplets, and cooling said droplets to rigid solid pellets of dry sarcosinate.
2. A containuous process for heat drying of fluid aqueous' solution of a normally solid rigid higher fatty acid sarcosinate as set forth in claim 1 in which the solution is moved turbulently as a wiped layer.
3. A continuous process for heat drying of fluid aqueous solution of a normally rigid solid higher fatty acid sarcosinate as set forth in claim 1 in which the solution is caused to move turbulently by frequent changes in cross sectional area as it flows between adjacent heating areas of said metallic surface.
4. A continuous process for converting an aqueous solution of sodium N-lauroyl sarcosinate at a solids concentration within the range of about to 40% into solid pellets having a moisture content not exceeding about 6% as set forth in claim 3 in which said stream is a thin wiped cylindrical layer and the vapor is separated countercurrently tosaid moving stream of solution as it is formed.
5. A continuous process for converting an aqueous solution of sodium N-lauroyl sarcosinate at a solids concentration within the range of about 10% to 40% into solid pellets having a moisture content not exceeding about 6% as set forth in claim 3 in which said stream frequently changes in direction and cross-section and the vapor and dried molten sarcosinate move concurrently until they are separated and the separation takes place by centrifugal action.
6. A continuous process for converting an aqueous solution of sodium N-lauroyl sarcosinate at a solids concentration within the range of about 10% to 40% into solid pellets having a moisture content not exceeding about 6% which comprises moving a stream of said solution continuously through a passageway, agitating and.
rapidly heating said solution as it moves through said passageway to a temperature within the range of about 145 to 195 C. for a period on the order of less than 2 minutes whereby aqueous solvent is converted into vapor until not more than 6% moisture is present in the sarcosinate and the thus dried sarcosinate is in molten conditi'on, separating said dried molten sarcosinate from said vapor before contact with any substantial amount of gas other than said vapor, forming said separated dried molten sarcosinate into discrete droplets, and cooling said drop lets to solid pellets of sodium N-lauroyl sarcosinate con; taining not over 6% moisture.
7. A'continuous process for heat drying, with minimum thermal decomposition, an aqueous higher fatty acid sarcosinate salt which is normally a rigid solid'comprising forming a flowable non-gelled aqueous solution of a normally solid higher fatty acid sarcosinate salt havinga tendency to gel when in aqueous solution at high concentration, disposing said flowable sarcosinate solution as a'wiped liquid film, turbulently agitating and I rapidly heating said film of sarcosinate solution to a'temperature. aboveboth'the boiling point of the solution forming said film and the melting point of said higher fatty acid sarcosinate salt, vaporizing substantially all of the water in said film to produce said higher fatty acid sarcosinate in molten, substantially dry form, forming droplets of said sarcosinate and immediately cooling said droplets to a temperature below its melting point to form higher fatty acid sarcosinate salt in the form of rigid, substantially dry, non-tacky pellets substantially free of any thermal degradation product.
8. A continuous process for heat drying an aqueous higher fatty acid sarcosinate as set forth in claim 7 wherein said sarcosinate is sodium N-lauroyl sarcosinate.
9. A continuous process for heat drying, with minimum decomposition, an aqueous higher fatty acid sarcosinate which is normally a rigid solid comprising forming, at a temperature below C., an aqueous solution containing from about 10 to 40% by weight of a higher fatty acid sarcosinate, said fatty acid being a straight chain monocarboxylic acid containing from 12 to- 16 carbon atoms, disposing said solution as a wiped liquid film less than inch thick on a heated metallic surface, turbulently agitating and rapidly heating said film to a temperature above the melting point of said sarcosinate for a period of from 10 to 30 seconds sufiicient to boil oif substantially all of the water therein and produce said higher fattyacid sarcosinate in molten, substantially dry fornn forrning droplets of said sarcosinate and immediately cooling said droplets to a temperature below about 40 C. to produce hi her fatty acid sarcosinate in the form of rigid, substantially dry, non-tacky pellets substantially free of any pyrolytic degradation product.
10. A continuous process for heat drying an aqueous solution of a normally rigid solid higher fatty acid sarcosinate which comprises moving turbulently a wiped layer of a fluid aqueous solution thereof over a heated surface, heating said layer to a temperature above both the boiling point of said solution and the melting point of said fatty acid sarcosinate, vaporizing substantially all of the water in said layer and melting the substantially dry fatty acid sarcosinate thus formed, forming said molten fatty acid sarcosinate into discrete liquid droplets, and cooling said droplets to rigid solid pellets of dry, higher fatty acid sarcosinate.
11. A continuous process for heat drying an aqueous solution of a higher fatty acid sarcosinate as set forth in claim 10 wherein said higher fatty acid sarcosinate is sodium N-lauroyl sarcosinate.
12. A continuous process for heat drying an aqueous solution of a higher fatty acid sarcosinate as set forth in claim 10 wherein said higher fatty acid sarcosinate is sodium N-palmitoyl sarcosinate.
' References Cited in the file of this patent UNITED STATES PATENTS 788,446 Wilson Apr. 25, 1905 868,447 Just Oct. 15, 1907 1,165,677 King Dec. 28, 1915 1,837,702 Canfield Dec. 22, 1931 2,341,258 Appel Feb. 8, 1944 2,643,180 Miller June 23, 1953 2,751,338 Schwemberger June 19, 1956 2,812,019 Rasmussen Nov. 5, 1957 2,817,155 Gilliam et al. Dec. 24, 1957 2,830,064 Monick Apr. 8, 1958 2,844,607 Gushin et al. July 22, 1958 2,863,888 Schurman Dec. 9, 1958 2,873,799 Barley et al. Feb. 17, 1959 2,890,155 Bueche June 9, 1959 FOREIGN PATENTS 740,825 Great Britain Nov. 23, 1955

Claims (1)

1. A CONTINUOUS PROCESS FRO HEAT DRYING OF FLUID AQUEOUS SOLUTION OF A NORMALLY RIGID SOLID HIGHER FATTY ACID SARCOSINATE WHICH COMPRISES MOVING SUCH SOLUTION TURBULENTLY OVER A HEATED METALLIC SURFACE IN DIRECT CONTACT THEREWITH, HEATING SAID SOLUTION THERBY TO A TEMPERATURE ABOVE BOTH THE BOILING POINT OF THE SOLUTION AND THE MELTING POINT OF THE SARCOSINATE, VAPORIZING SUBSTANTIALLY ALL OF THE AQUEOUS SOLVENT FROM SAID SOLUTION AND MELTING THE SUBSTANTIALLY DRY SARCOSINATE THUS FORMED BEFORE CONTACT WITH ANY SUBSTANTIAL AMOUNT OF GAS OTHER THAN SAID VAPOR, FORMING THE MOLTEN DRIED SARCOSINATE INTO DISCRETE LIQUID DROPLETS, AND COOLING SAID DROPLETS TO RIGID SOLID PELLETS FO DRY SARCOSINATE.
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US3290153A (en) * 1964-09-18 1966-12-06 Schlitz Brewing Co J Process and apparatus for concentrating wort
US3397730A (en) * 1965-12-21 1968-08-20 Gen Electric Liquid feed distributor
US3521691A (en) * 1969-01-06 1970-07-28 Artisan Ind Multistaged moving film and wiped film evaporators
WO1984001022A1 (en) * 1982-09-02 1984-03-15 Superstill Technology Inc An improved method and apparatus for recycling energy in counterflow heat exchange and distillation
US4869067A (en) * 1982-09-02 1989-09-26 Superstill Corporation Method of generating power
US20070208200A1 (en) * 2006-03-01 2007-09-06 Kenny Randolph Parker Methods and apparatus for producing a low-moisture carboxylic acid wet cake
US20070208196A1 (en) * 2006-03-01 2007-09-06 Kenny Randolph Parker Method and apparatus for drying carboxylic acid
US20220401328A1 (en) * 2021-06-08 2022-12-22 The Procter & Gamble Company N-acyl amino acid surfactants and derivatives thereof

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US8697906B2 (en) 2006-03-01 2014-04-15 Grupo Petrotemex, S.A. De C.V. Methods and apparatus for producing a low-moisture carboxylic acid wet cake
US20220401328A1 (en) * 2021-06-08 2022-12-22 The Procter & Gamble Company N-acyl amino acid surfactants and derivatives thereof

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