US3190900A - Continuous process for soap washing - Google Patents

Continuous process for soap washing Download PDF

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Publication number
US3190900A
US3190900A US178829A US17882962A US3190900A US 3190900 A US3190900 A US 3190900A US 178829 A US178829 A US 178829A US 17882962 A US17882962 A US 17882962A US 3190900 A US3190900 A US 3190900A
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United States
Prior art keywords
soap
lye
washing
glycerol
column
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Expired - Lifetime
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US178829A
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English (en)
Inventor
Godet Pierre
Gachon Rene
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Colgate Palmolive Co
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Colgate Palmolive Co
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Publication date
Application filed by Colgate Palmolive Co filed Critical Colgate Palmolive Co
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
    • C11D13/02—Boiling soap; Refining
    • C11D13/04—Continuous methods therefor

Definitions

  • the present invention relates to the manufacture of soap and more particularly to the extraction of glycerol and impurities from soap produced by the saponification of fats and oils.
  • the first stage of soap manufacture consists of a chemical reaction called saponification.
  • the products of this reaction are soap and glycerol.
  • this crude mixture also contains various impurities resulting either from the raw materials used or from secondary reactions accompanying the saponification reaction.
  • the crude soap must, therefore, undergo washings in order to remove to glycerol and the impurities.
  • These washings are generally madewith alkali or alkaline lye solutions whose electrolyte concentration is higher than the concentration at which the soap begins to be soluble in the lye. This is called the limit lye.
  • the soap phase is in fact formed by a pure soap hydrate containing 66% of fatty acids and a lye identical in composition to the one which separates from it.
  • the glycerol which has to be extracted by washing is not retained in solution in thesoap phase, but is dissolved in the lye mixed with the soap.
  • a division coefiicient of the glycerol between the soap phase and the lye phase does not exist due to the fact that the amount of glycerol retained in the soap depends onthe quantity of lye that it retains, and which according to the conditions is highly variable.
  • the soap phase obtained after saponification is divided into very small grains, their coalesence into a single body does not occur before the passage of a relatively long time, i.e., approximately 30 minutes, even if these grains are brought into contact.
  • This time has been found to be sufiicient to permit the replacement of the glycerin-like lye, contained in the soap grains which are to be washed, by fresh lye, thus extracting the glycerol and the impurities which accompany it from the soap grains.
  • the size of the grains of soap will determine the ease of the lye replacement operation.
  • the grains should have a volume'of less than 100 cubic millimeters.
  • a process for extracting impurities and glycerol from crude soap comprises introducing countercurrently a washing lye and a crude soap containing said impurities and glycerol into a washing zone, pulsing the washing lye-crude soap mixture in the washing zone while simultaneously reducing and expanding cross-sectional areas of the washing lye-crude soap mixture at intervals along the length of the washing zone, and collecting the washed soap and the washing lye containing said impurities and glycerol in separately spaced settling zones.
  • the instant invention relates to a continuous soap washing process, which comprises introducing continuously and countercurrently a washing lye phase and a crude soap phase containing impurities and glycerol into a column equipped with perforated plates arranged in tiers, the crude soap, forming the upwards flowing phase, setting the liquid in the column into reciprocating motion adapted to effect the passage of the soap phase through the perforations of the plates in the form of small grains or droplets thereof, and continuously collecting washed soap and washing lye containing substantially all of said soap impurities and glycerol in settling zones disposed at the top and the bottom of the column respectively.
  • the function of the perforated plates in the practice of this invention is believed to be basically different fromv the function which they play in a liquid-liquidextraction column. In the latter instance, they are redispersion elements of a dispersed phase which has a tendency to coalesce quickly.
  • the function of the plates is to break and to deform increasingly the soap grains in order to remove the lye impurity and to replace it with a'washing lye having a smaller content of impurities and glycerol.
  • cross-sectional areas of the washing lye-crude soap mixture are simultaneously reduced (in the perforated plates) and expanded (in the zones between the perforated plates).
  • the apparatus of the invention does not require the use of a circulation pump between the entrance and exit of soap, or any mixing device.
  • the perforated plates are permanent, simple, non-mechanical devices which do not require any maintenance.
  • Another advantage of the process of this invention resides in the fact that the apparatus is entirely closed. This is particularly advantageous with respect to the quality of the soap obtained, since no oxidation can take place by contact with air. Since the materials remain in the column only a very short time, it is not necessary to heat the column and, therefore, the steam consumption of the process is accordingly reduced to a minimum. Moreover, the simplicity of operating a column requires only a minimum of labor. Even manual intervention is not required as a simple and conventional automatic control can be easily adopted.
  • a device 7 which can be a piston pump (as shown), a pneumatic device or any other device imparting to the materials contained in the column an alternative or reciprocating motion upwards and downwards.
  • the body of the column comprises in the interior, horizontal plates or discs 2, 3, 4, 5, 6, etc., perforated with holes or openings.
  • the diameter of the holes can vary from 1 to 10 mm., but preferably should be from 2 to 6 mm.
  • the number of holes per unit of surface of the discs can vary in such a way that the percentage of free passage through a disc comprises between and 50%.
  • the spacing between the discs depends on several factors such as the required efiiciency, the flooding limits, the pulsation characteristics, etc. This spacing can preferably vary from 2 to 20 cm.
  • the diameter of the column depends on the required production capacity. Different inlet and outlet pipes are connected to this column, as can be seen hereafter in the explanation of the operation.
  • the soap to be washed, coming from the saponification stage, is introduced in inlet 10.
  • inlet 11 the washing lye is introduced, the composition of which as regards caustic and salt contents is such that the soap coming out at the top has the desired minimum content of. cautsic and salt.
  • the soap introduced in conduit or inlet 10 thus flow upwards from inlet 10 to outlet 12 and meets the lye entering at inlet 11 and discharging at outlet 13, the latter thereby washing the soap countercurrently.
  • Settling section 8 allows separation, through settling, of the lye from the soap which is to be washed, this lye being removed at outlet 13.
  • the settling section 9 is de signed to separate the lye from the washed soap. The latter is removed at outlet 12.
  • the volumes of the settling sections are such that they allow a sufficient settling time for the separation of the lye from the soap. This settling time can vary from 10 to 60 minutes.
  • the diameter of the settling sections should be preferably larger than that of the column, for example, fromlO to 50% larger, as is customary in the construction of extraction columns.
  • Pulsation i.e. the reciprocating displacement, imparted to the liquid of the column by the piston device 7 is characterized by its frequency and the amplitude of displacement of the liquid in the column. Expedient values for these characteristics have been found to be as follows:
  • Example I A 120 cm. diameter column, having a configuration as illustrated in FIG. 1, 5.7 meters high and whose packing was formed by 46 discs perforated with 50,000 3 mm. holes, was pulsated at the rate of 150 strokes per minute with an amplitude of 6.5 mm. of displacement of liquid in the column.
  • This column was fed at the base with 6000 kg. per hour of sodium soap obtained through saponification of a mixture of tallow and 15% coconut oil at a temperature of 80 to C.
  • the soap contained 3.7% glycerol.
  • Three thousand (3,000) kg. per hour of a washing lye was fed into the column at a temperature of from 80 to 103 C. This lye contained 6.3% salt and 2.1% caustic so a.
  • Example 2 A 40 cm. diameter column, having a configuration as illustrated in FIG. 1, 4.8 meters high whose packing was formed by 28 discs perforated with 4000 4 mm. holes, was pulsated at the rate of 180 strokes per minute with a 10 mm. displacement amplitude of the liquid in the column.
  • This column was fed at the lower inlet with 650 kg. per hour of sodium soap, obtained through saponification of a mixture of 40% tallow, 12% coconut oil, 36% fat and 12% rosin at a temperature of 80 to 90 C.
  • the soap contained 4% glycerol.
  • washing lye was fed into the column at the rate of 350 kg. per hour through the upper inlet. This lye contained 8.2% salt and 1.8% caustic soda. The electrolyte concentration of this lye was higher than the concentration of limit lye.
  • the washed soap exiting from the top outlet of the column has a glycerol content of .2%.
  • Example 3 A 70 cm. diameter column, having a configuration as illustrated in FIG. 1, 4 meters high and whose packing was formed by 50 discs perforated with 5000 5 mm. holes was pulsated at the rate of 120 strokes per minute with a 5 mm. displacement amplitude of the liquid in the column.
  • This column was fed at the base with 2000 kg. per hour of sodium soap obtained through saponification of a mixture of 80% peanut oil and 20% coconut oil at a temperature of 90 C. This mixture contained 5% glycerol.
  • the washed soap exiting from the top outlet of the column had a glyceral content of 0.4%.
  • Example 4 A 50 cm. diameter column, having a configuration as illustrated in FIG. 1, 7 meters high and whose packing was formed by 45 discs perforated with 2650 6 mm. holes was pulsated at the rate of 200 strokes per minute with a 3 mm. displacement amplitude of the liquid in the column.
  • This column was fed at the base with 1000 kgs. per hour of a sodium soap obtained through saponification of a mixture of 60% tallow, 20% palm oil and 20% cabbage palm oil at a temperature of 95 C.
  • This soap contained 5.7% of glycerol.
  • the soap coming out at the upper part of the column contained 0.07% glycerol.
  • Example 5 A 50 cm. diameter column, 5 meters high and whose packing was formed by 40 discs perforated with 28,000 3 mm. holes was pulsated at the rate of 100 strokes per minute with a 7 mm. displacement amplitude of the 7 liquid in the column.
  • This column was fed at its lower inlet with 3500 kgs. per hour of a potassium soap at 90 C. obtained through saponification of olive oil. This soap contained 5.2% glycerol.
  • the washing lye fed into the column at the rate of 1800 kgs. per hour through the upper inlet of the column was a solution containing 12% of potassium chloride. This concentration was higher than the limit lye concentration.
  • a process for extracting impurities and glycerol from crude soap which comprises introducing countercurrently a washing lye and a crude soap containing said impurities and glycerol into a columnar washing zone, said crude soap forming the upwards flowing phase, pulsing the washing lye-crude soap mixture in the washing zone to impart a reciprocating motion to said mixture while simultaneously reducing and expanding cross-sectional areas of the washing lye-crude soap mixture at intervals along the length of the washing zone by means of a plurality of perforated plates arranged in tiers, said soap of said mixture being thereby reduced in particle size .and collecting washed soap and washing lye containing substantially all of said impurities and glycerol in separately spaced settling zones disposed at the top and the bottom respectively of the washing zone.
  • a continuous process for extracting impurities and glycerol from crude soap which comprises continuously introducing countercurrently a washing lye and a crude soap containing said impurities and glycerol into a columnar washing zone, the crude soap forming the upwards flowing phase; continuously pulsing the washing lyecrude soap mixture in the washing zone to impart a reciprocating motion to said mixture while simultaneously reducing and expanding cross-sectional areas of the washing lye-crude soap mixture at a plurality of intervals along the length of the washing zone by means of a plurality of perforated plates arranged in tiers, said soap of said mixture being thereby reduced in particle size, and continuously collecting washed soap and washing lye containing substantially all of said impurities and glycerol in settling zones disposed at the top and the bottom respectively of the washing zone.
  • washing lye has a concentration of about the limit lye.
  • washing lye has a concentration of slightly below the limit lye.
  • a continuous process for extracting impurities and glycerol from crude soap which comprises introducing continuously and countercurrently a washing lye phase and a crude soap phase containing said impurities and glycerol into a washing zone fitted with'a plurality of perforated plates arranged in tiers, the crude soap forming the upwards flowing phase, pulsing the washing lyecrude soap mixture in the washing zone to impart a reciprocating motion to said mixture and to effect passage of the soap phase through the perforations of the plates in the form of small grains thereof, and continuously collecting washed soap. and washing lye containing substantially all of said impurities and glycerol in settling zones disposed at the top and bottom respectively of the washing zone.
  • washing lye has a concentration of about the limit lye.
  • washing lye has a concentration of slightly below the limit lye.
  • a continuous process for extracting impurities and glycerol from crude soap which comprises introducing continuously and countercurrently a washing lye phase and a crude soap phase containing said impurities and glycerol into a washing zone fitted with a plurality of perforated plates arranged in tiers :spaced 2 to 20 cm.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
US178829A 1961-03-23 1962-03-12 Continuous process for soap washing Expired - Lifetime US3190900A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR856582A FR1337212A (fr) 1961-03-23 1961-03-23 Procédé continu de lavage du savon et appareil pour sa mise en oeuvre

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US3190900A true US3190900A (en) 1965-06-22

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US178829A Expired - Lifetime US3190900A (en) 1961-03-23 1962-03-12 Continuous process for soap washing

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US (1) US3190900A (US20080293856A1-20081127-C00150.png)
BE (1) BE614628A (US20080293856A1-20081127-C00150.png)
CH (1) CH415917A (US20080293856A1-20081127-C00150.png)
DE (1) DE1223093C2 (US20080293856A1-20081127-C00150.png)
FR (1) FR1337212A (US20080293856A1-20081127-C00150.png)
GB (1) GB989745A (US20080293856A1-20081127-C00150.png)
NL (1) NL275152A (US20080293856A1-20081127-C00150.png)
OA (1) OA00854A (US20080293856A1-20081127-C00150.png)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2549386A1 (fr) * 1983-07-21 1985-01-25 Colgate Palmolive Co Appareil et procede d'extraction continue au moyen d'un liquide non miscible
US4668398A (en) * 1983-07-21 1987-05-26 Colgate-Palmolive Company Continuous extraction apparatus and process

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3047995B1 (fr) 2016-02-19 2020-01-03 Rampal Patou Procede de fabrication de savon

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2562207A (en) * 1946-01-21 1951-07-31 Lever Brothers Ltd Continuous method of washing soap

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1069319B (US20080293856A1-20081127-C00150.png) * 1959-11-19

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2562207A (en) * 1946-01-21 1951-07-31 Lever Brothers Ltd Continuous method of washing soap

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2549386A1 (fr) * 1983-07-21 1985-01-25 Colgate Palmolive Co Appareil et procede d'extraction continue au moyen d'un liquide non miscible
DE3425846A1 (de) * 1983-07-21 1985-01-31 Colgate-Palmolive Co., New York, N.Y. Extraktionsapparat und verfahren zum kontinuierlichen extrahieren
US4571299A (en) * 1983-07-21 1986-02-18 Colgate-Palmolive Company Continuous extraction apparatus
US4668398A (en) * 1983-07-21 1987-05-26 Colgate-Palmolive Company Continuous extraction apparatus and process

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DE1223093C2 (de) 1975-02-13
NL275152A (US20080293856A1-20081127-C00150.png)
OA00854A (fr) 1967-11-15
FR1337212A (fr) 1963-09-13
DE1223093B (de) 1975-02-13
GB989745A (en) 1965-04-22
BE614628A (US20080293856A1-20081127-C00150.png)
CH415917A (fr) 1966-06-30

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