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US4322367A
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Deoiling of aqueous solutions of sodium lauryl sulfate
Assignee: Colgate Palmolive Co
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Filing: 1979-11-26
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Granted: 1982-03-30
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Expires: 1999-11-26
Abstract
Abstract Free oil, often an objectionable impurity in synthetic organic detergents, such as sodium lauryl sulfate, is removed from aqueous solutions by extraction thereof with hexane in the presence of lower alkanol, with the proportion of the alkanol present being in a relatively narrow range with respect to the sodium lauryl sulfate, in which range it helps to promote efficient extraction of the free oil by the hexane without solubilizing the hexane in the aqueous medium to such an extent as to result in an extracted detergent containing an unacceptably high proportion of hexane. Separation of the free oil from the aqueous detergent solution is effected in an extractor, to which the hexane is added, in mixture with a minor proportion of lower alkanol, normally isopropanol, and extraction of the free oil takes place after a preliminary mixing of isopropanol with detergent acid or neutralized base in a neutralization vessel and/or in a mixer upstream of the extractor. In a preferred embodiment of the invention the hexane extractant feed to the extractor is that resulting from distillation separation from the free oil of the hexane with some isopropanol. Also, extracted product is evaporated and the evaporator overhead, including isopropanol, hexane and water, is fed to the mixer. The evaporator product is steam stripped, very preferably in a novel stripper described herein, and the stripper overhead, including isopropanol and water, is conveniently fed to a neutralization vessel in which detergent acid, comprising the product of sulfation of lauryl alcohol with sulfur trioxide (and containing objectionable free oil), is neutralized with aqueous sodium hydroxide. Preferably the deoiling process is a continuous one, with only free oil being removed from the extractor feed, and the hexane and isopropanol are continuously recycled.
Inventors
- 👤 Salvatore J. Silvis
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 21:00
CPC Classifications
B; B01; B01D; B01D3/00; B01D3/08; B01D3/14; B01D3/16; B01D3/18; B01D3/20; B01D3/34; B01D3/40; C; C07; C07C; C07C303/00; C07C303/42; C07C303/44; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/582
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
378 words
A method for deoiling a water-soluble salt of a C 10 -C 18 alkyl sulfate detergent in an aqueous medium containing oil therein which comprises the steps of admixing an aqueous detergent containing 25% to 33% by weight of said sulfate detergent and 1% to 6% of oil to be removed with a mixture of C 1 -C 3 aliphatic alcohol, C 4 -C 9 hydrocarbon and water to form a single-phase liquid containing said detergent, said oil, water, C 1 -C 3 aliphatic alcohol and C 4 -C 9 hydrocarbon in which the weight ratio of aliphatic alcohol to said detergent is within the range of 1.3:1 to 2.5:1 by weight; contacting said single-phase liquid detergent solution from the preceding step with an extractant solution containing liqiud C 1 -C 3 aliphatic alcohol and a liquid C 4 -C 9 hydrocarbon, said extractant solution being in substantial equilibrium with said liquid detergent solution except for the oil content thereof so as to extract oil from said single-phase detergent liquid without significantly altering the balance of the composition of said detergent solution; separating such liquids into two portions substantially corresponding to those before contacting is effected, with C 4 -C 9 hydrocarbon, C 1 -C 3 alcohol and free oil in the first portion and alkyl sulfate, C 1 -C 3 alcohol, water and C 4 -C 9 hydrocarbon in the second portion; separating the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol from the free oil of said first portion; evaporating said second portion material to remove portions of C 1 -C 3 alcohol, C 4 -C 9 hydrocarbon and water therefrom and to increase the concentration of said alkyl sulfate salt in the aqueous solution thereof; stripping C 1 -C.sub. 3 alcohol from the concentrated alkyl sulfate solution resulting; returning the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol after removal of free oil therefrom back to the extraction step; adding the C 1 -C 3 alcohol, C 4 -C 9 hydrocarbon and water mixture removed from the extracted detergent solution back to said aqueous detergent solution prior to extraction thereof; and recycling the C 1 -C 3 alcohol stripped off the detergent solution to another step of this method.
Claim 2
Independent Claim
378 words
A method for deoiling a water-soluble salt of a C 10 -C 18 alkyl sulfate detergent in an aqueous medium containing oil therein which comprises the steps of admixing an aqueous detergent containing 25% to 33% by weight of said sulfate detergent and 1% to 6% of oil to be removed with a mixture of C 1 -C 3 aliphatic alcohol, C 4 -C 9 hydrocarbon and water to form a single-phase liquid containing said detergent, said oil, water, C 1 -C 3 aliphatic alcohol and C 4 -C 9 hydrocarbon in which the weight ratio of aliphatic alcohol to said detergent is within the range of 1.3:1 to 2.5:1 by weight; contacting said single-phase liquid detergent solution from the preceding step with an extractant solution containing liqiud C 1 -C 3 aliphatic alcohol and a liquid C 4 -C 9 hydrocarbon, said extractant solution being in substantial equilibrium with said liquid detergent solution except for the oil content thereof so as to extract oil from said single-phase detergent liquid without significantly altering the balance of the composition of said detergent solution; separating such liquids into two portions substantially corresponding to those before contacting is effected, with C 4 -C 9 hydrocarbon, C 1 -C 3 alcohol and free oil in the first portion and alkyl sulfate, C 1 -C 3 alcohol, water and C 4 -C 9 hydrocarbon in the second portion; separating the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol from the free oil of said first portion; evaporating said second portion material to remove portions of C 1 -C 3 alcohol, C 4 -C 9 hydrocarbon and water therefrom and to increase the concentration of said alkyl sulfate salt in the aqueous solution thereof; stripping C 1 -C.sub. 3 alcohol from the concentrated alkyl sulfate solution resulting; returning the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol after removal of free oil therefrom back to the extraction step; adding the C 1 -C 3 alcohol, C 4 -C 9 hydrocarbon and water mixture removed from the extracted detergent solution back to said aqueous detergent solution prior to extraction thereof; and recycling the C 1 -C 3 alcohol stripped off the detergent solution to another step of this method.
Claim 3
Independent Claim
296 words
A method of deoiling a water-soluble salt of a sulfonated or sulfated anionic detergent having an alkyl group of 8 to 20 carbon atoms in its molecular structure in an aqueous medium containing oil therein which comprises the steps of admixing an aqueous detergent containing 25% to 33% by weight of said detergent and 1% to 6% of oil to be removed with a mixture of C 1 -C 3 aliphatic alcohol, C 4 -C 9 hydrocarbon and water to form a single-phase liquid containing said detergent, said oil, water, C 1 -C 3 aliphatic alcohol and C 4 -C 9 hydrocarbon in which the weight ratio of aliphatic alcohol to said detergent is within the range of 1.3:1 to 2.5:1 by weight, contacting said single-phase liquid detergent solution from the preceding step with an extractant solution containing liquid C 1 -C 3 aliphatic alcohol and a liquid C 4 -C 9 hydrocarbon, said extractant solution being in substantial equilibrium with said detergent solution except for the oil content thereof so as to extract oil from said single-phase detergent liquid without significantly altering the balance of the composition of said detergent solution; separating such liquids into two portions substantially corresponding to those before contacting is effected, with C 4 -C 9 hydrocarbon, C 1 -C 3 alcohol and free oil in the first portion and anionic salt, C 1 -C 3 alcohol, water and C 4 -C 9 hydrocarbon in the second portion; separating the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol from the free oil of said first portion; and recycling said recovered mixture of C 1 -C 3 alcohol and C 4 -C 9 hydrocarbon to said extraction step for use in extracting oil from additional aqueous anionic detergent salt.
Claim 4
Independent Claim
296 words
A method of deoiling a water-soluble salt of a sulfonated or sulfated anionic detergent having an alkyl group of 8 to 20 carbon atoms in its molecular structure in an aqueous medium containing oil therein which comprises the steps of admixing an aqueous detergent containing 25% to 33% by weight of said detergent and 1% to 6% of oil to be removed with a mixture of C 1 -C 3 aliphatic alcohol, C 4 -C 9 hydrocarbon and water to form a single-phase liquid containing said detergent, said oil, water, C 1 -C 3 aliphatic alcohol and C 4 -C 9 hydrocarbon in which the weight ratio of aliphatic alcohol to said detergent is within the range of 1.3:1 to 2.5:1 by weight, contacting said single-phase liquid detergent solution from the preceding step with an extractant solution containing liquid C 1 -C 3 aliphatic alcohol and a liquid C 4 -C 9 hydrocarbon, said extractant solution being in substantial equilibrium with said detergent solution except for the oil content thereof so as to extract oil from said single-phase detergent liquid without significantly altering the balance of the composition of said detergent solution; separating such liquids into two portions substantially corresponding to those before contacting is effected, with C 4 -C 9 hydrocarbon, C 1 -C 3 alcohol and free oil in the first portion and anionic salt, C 1 -C 3 alcohol, water and C 4 -C 9 hydrocarbon in the second portion; separating the C 4 -C 9 hydrocarbon and C 1 -C 3 alcohol from the free oil of said first portion; and recycling said recovered mixture of C 1 -C 3 alcohol and C 4 -C 9 hydrocarbon to said extraction step for use in extracting oil from additional aqueous anionic detergent salt.
Claim 5
Dependent Claim
22 words
A method according to claim 1 wherein the first and second portions are upper and lower body portions, respectively, in an extractor.
Claim 6
Dependent Claim
67 words
A method according to claim 3 wherein the composition of the detergent solution for extraction is adjusted in a mixer before the extractor by mixing neutralized base, comprising said alkyl sulfate, free oil, water and C 1 -C 3 alcohol, with a mixture of C 1 -C 3 alcohol, C 4 -C 9 hydrocarbon and water recovered from evaporation of the second portion from the extraction step.
Claim 7
Dependent Claim
24 words
A method according to claim 4 wherein the temperature of the mixture in the extractor is in the range of 15° to 70° C.
Claim 8
Dependent Claim
79 words
A method according to claim 5 wherein said alkyl sulfate is sodium lauryl sulfate, said C 1 -C 3 alcohol is isopropanol, said C 4 -C 9 hydrocarbon is hexane, the temperature of the mixture in the extractor is in the range of 30° to 35° C., and the hexane and isopropanol are distilled off from the free oil at a temperature in the range of 65° to 90° C. and at a pressure of 0.9 to 1.1 atmosphere.
Claim 9
Dependent Claim
83 words
A method according to claim 6 wherein the concentration of sodium lauryl sulfate in the evaporator product is 27 to 37% by weight, isopropanol, hexane and water, removed from the evaporator separate from the evaporated product, are mixed with the aqueous solution of sodium lauryl sulfate before extraction of free oil therefrom, to produce a solution that is immiscible with and in equilibrium with the extractant, and the concentration of sodium lauryl sulfate in the stripper product is 25 to 35% by weight.
Claim 10
Dependent Claim
30 words
A method according to claim 7 wherein the temperatures and pressures in the evaporator and stripper are within the range of 25° to 100° C. and 150 to 350 torr.
Claim 11
Dependent Claim
48 words
A method according to claim 8 wherein the aqueous solution of sodium lauryl sulfate being deoiled contains from 3.2 to 19.4 parts of free oil per hundred parts of sodium lauryl sulfate and from 1 to 9.7 parts of sodium sulfate per hundred parts of sodium lauryl sulfate.
Claim 12
Dependent Claim
51 words
A method according to claim 9 wherein the sodium lauryl sulfate being deoiled is that resulting from sulfur trioxide sulfation of lauryl alcohol and neutralization by sodium hydroxide of the sulfuric reaction product made, and the free oil being removed from the sodium lauryl sulfate is that resulting from such reactions.
Claim 13
Dependent Claim
23 words
A method according to claim 10 wherein evaporation of the lower body portion material from the extractor is effected in a wiped-film evaporator.
Claim 14
Dependent Claim
98 words
A method according to claim 1 wherein the concentrated alkyl sulfate solution is countercurrently steam stripped in a stripping column having a plurality of contacting zones therein, with steam being admitted to said column near one end thereof, mixed consecutively with different portions of aqueous solution of product to be stripped, consecutively separated from such portions of liquid, and passed out near the other end of the column, enriched in isopropanol, and with such solution being stripped passing through the column in an opposite direction, to be consecutively contacted by such steam or vapor of lower isopropanol content.
Claim 15
Dependent Claim
99 words
A method according to claim 11 wherein the liquid lauryl sulfate evaporator product is countercurrently steam stripped in a stripping column having a plurality of contacting zones therein, with steam being admitted to said column near one end thereof, mixed consecutively with different portions of aqueous solution of product to be stripped, consecutively separated from such portions of liquid, and passed out near the other end of the column, enriched in isopropanol, and with such solution being stripped passing through the column in an opposite direction, to be consecutively contacted by such steam or vapor of lower isopropanol content.
Claim 16
Dependent Claim
9 words
A method according to claim 1, which is continuous.
Claim 17
Dependent Claim
64 words
A method according to claim 13 wherein the steam and water-isopropanol vapor generated by it move upwardly through the column and detergent solution to be stripped moves downwardly through it, with the flow of the steam or the water-isopropanol vapor repeatedly drawing into contact with it liquid to be stripped and with such liquid-vapor mixtures made being repeatedly separated into liquid and vapor streams.
Claim 18
Dependent Claim
57 words
A method according to claim 2 wherein the aqueous medium containing anionic salt and oil therein is one which intially is not in equilibrium with the extractant solvent and which is converted to a solution in equilibrium therewith by addition to it of such C 1 -C 3 aliphatic alcohol and liquid C 4 -C 9 hydrocarbon.
Claim 19
Dependent Claim
55 words
A method according to claim 16 wherein the synthetic detergent of the detergent solution is sodium lauryl sulfate, the lower aliphatic alcohol is isopropanol, the liquid hydrocarbon is hexane and the isopropanol and hexane added to the detergent solution to bring it into equilibrium with the extractant liquid are added as a mixture containing water.
References Cited (Backward Citations)
US3865861A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-03-29 | 1985-09-28 | 1986-03-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-03-29 | 1989-09-28 | 1990-03-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-03-29 | 1993-09-28 | 1994-03-30 | $7700.00 | Window Closed / Lapsed |