Patent US5290484A successfully refreshed from Google Patents.
US5290484A
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US
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Process for the preparation of secondary alkyl sulfate-containing surfactant compositions
Assignee: Shell USA Inc
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Filing: 1992-11-12
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Granted: 1994-03-01
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Expires: 2012-11-12
Abstract
Abstract This invention relates to a process for preparing solid and non-solid secondary alkyl sulfate-containing surface active compositions. The solid secondary alkyl sulfate-containing surface active compositions are formed by crystallization, and the non-solid secondary alkyl sulfate-containing surface active compositions are recovered in a glycol solvent. These compositions are substantially free of unreacted organic matter and water.
Inventors
- 👤 Eugene F. Lutz
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 21:51
CPC Classifications
C; C11; C11D; C11D1/00; C11D1/02; C11D1/12; C11D1/14; C11D1/146; C07; C07C; C07C303/00; C07C303/24; C07C303/42; C07C303/44; Y; Y10; Y10S; Y10S516/00; Y10S516/01; Y10S516/03
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
146 words
A process for preparing secondary alkyl sulfate-containing surface active compositions which comprises: a) preparing a detergent range alkyl sulfuric acid-containing solution, b) contacting said detergent range alkyl sulfuric acid-containing solution with a base in aqueous solution, c) heating the product of step b) to saponify dialkyl sulfate and to remove substantially all of the water from the reaction- mixture, d) cooling the product of step c) in the presence of a nonionic organic liquid diluent to crystallize a solid secondary alkyl sulfate-containing surface active composition from the reaction mixture and recovering therefrom a crystallized solid secondary alkyl sulfate-containing surface active composition, e) contacting and mixing the uncrystallized portion of the product of step d) with a glycol, and f) phase separating the mixture of step e) into an upper phase product and a lower phase product which contains a non-solid secondary alkyl sulfate-containing surface active composition.
Claim 2
Dependent Claim
146 words
A process for preparing secondary alkyl sulfate-containing surface active compositions which comprises: a) preparing a detergent range alkyl sulfuric acid-containing solution, b) contacting said detergent range alkyl sulfuric acid-containing solution with a base in aqueous solution, c) heating the product of step b) to saponify dialkyl sulfate and to remove substantially all of the water from the reaction- mixture, d) cooling the product of step c) in the presence of a nonionic organic liquid diluent to crystallize a solid secondary alkyl sulfate-containing surface active composition from the reaction mixture and recovering therefrom a crystallized solid secondary alkyl sulfate-containing surface active composition, e) contacting and mixing the uncrystallized portion of the product of step d) with a glycol, and f) phase separating the mixture of step e) into an upper phase product and a lower phase product which contains a non-solid secondary alkyl sulfate-containing surface active composition.
Claim 3
Dependent Claim
38 words
The process of claim 1 wherein said detergent range alkyl sulfuric acid-containing solution is prepared by sulfating a reactant selected from the group consisting of detergent range olefins, detergent range alcohols and mixtures thereof, with a sulfating agent.
Claim 4
Dependent Claim
25 words
The process of claim 1 wherein the nonionic organic liquid diluent is selected from the group consisting of aliphatic hydrocarbons, aromatic hydrocarbons and mixtures thereof.
Claim 5
Dependent Claim
28 words
The process of claim 3 wherein the nonionic organic liquid diluent in step c) is selected from the group consisting of heptane, toluene, isooctane, nonane, and mixtures thereof.
Claim 6
Dependent Claim
25 words
The process of claim 1 wherein the base in step b) is selected from ammonium, alkali metal or alkaline earth metal hydroxides, carbonates or bicarbonates.
Claim 7
Dependent Claim
22 words
The process of claim 5 wherein said base is selected from the group consisting of sodium hydroxide, potassium hydroxide and mixtures thereof.
Claim 8
Dependent Claim
28 words
The process of claim 1 wherein said base in aqueous solution comprises from about 10 percent by weight to about 85 percent by weight of base in water.
Claim 9
Dependent Claim
41 words
The process of claim 1 wherein said solid secondary alkyl sulfate-containing surface active composition recovered in step d) contains from about 80 percent by weight to about 99 percent by weight secondary alkyl sulfate, basis the weight of recovered crystallized solid.
Claim 10
Dependent Claim
15 words
The process of claim 1 wherein said glycol in step e) is an alkyl glycol.
Claim 11
Dependent Claim
26 words
The process of claim 9 wherein said alkyl glycol is selected from the group consisting of 1,2-propanediol, diethylene glycol, ethylene glycol, 1,4-butanediol, glycerine and mixtures thereof.
Claim 12
Dependent Claim
47 words
The process of claim 1 wherein said lower phase product in step f) which contains a non-solid secondary alkyl sulfate-containing surface active composition contains from about 5 percent by weight to about 60 percent by weight secondary alkyl sulfate, basis the weight of the lower phase product.
Claim 13
Dependent Claim
140 words
A process for preparing secondary alkyl sulfate-containing surface active compositions substantially free of unreacted organic matter and water, which process comprises: a) sulfating a reactant selected from the group consisting of detergent range olefins, detergent range alcohols and mixtures thereof, b) neutralizing the sulfation product of step a) with a base in aqueous solution, c) saponifying the product of step b), d) crystallizing the product of step c) and recovering therefrom a crystallized solid secondary alkyl sulfate-containing surface active composition, e) contacting and mixing the uncrystallized portion of the product of step d) with a glycol, and f) phase separating the mixture of step e) into an upper phase product and a lower phase product which contains a non-solid secondary alkyl sulfate-containing surface active composition, wherein in said process, a nonionic organic liquid diluent is added prior to step d).
Claim 14
Dependent Claim
140 words
A process for preparing secondary alkyl sulfate-containing surface active compositions substantially free of unreacted organic matter and water, which process comprises: a) sulfating a reactant selected from the group consisting of detergent range olefins, detergent range alcohols and mixtures thereof, b) neutralizing the sulfation product of step a) with a base in aqueous solution, c) saponifying the product of step b), d) crystallizing the product of step c) and recovering therefrom a crystallized solid secondary alkyl sulfate-containing surface active composition, e) contacting and mixing the uncrystallized portion of the product of step d) with a glycol, and f) phase separating the mixture of step e) into an upper phase product and a lower phase product which contains a non-solid secondary alkyl sulfate-containing surface active composition, wherein in said process, a nonionic organic liquid diluent is added prior to step d).
Claim 15
Dependent Claim
22 words
The process of claim 12 wherein said reactant is a detergent range olefin having from about 12 to about 18 carbon atoms.
Claim 16
Dependent Claim
34 words
The process of claim 12 wherein said sulfating step is carried out using concentrated sulfuric acid having a concentration of from about 75 percent by weight to about 100 percent by weight in water.
Claim 17
Dependent Claim
42 words
The process of claim 12 wherein said sulfating step is carried out at a temperature in the range of from about 5° C. to about 40° C. and a pressure in the range of from about 1 atmosphere to about 2 atmospheres.
Claim 18
Dependent Claim
21 words
The process of claim 12 wherein following step a), the product of step a) is subjected to deacidification by water washing.
Claim 19
Dependent Claim
25 words
The process of claim 12 wherein said base in step b) is selected from ammonium, alkali metal or alkaline earth metal hydroxides, carbonates or bicarbonates.
Claim 20
Dependent Claim
22 words
The process of claim 17 wherein said base is selected from the group consisting of sodium hydroxide, potassium hydroxide and mixtures thereof.
Claim 21
Dependent Claim
27 words
The process of claim 12 wherein said base in aqueous solution comprises from about 10 percent by weight to about 85 percent by weight base in water.
Claim 22
Dependent Claim
42 words
The process of claim 12 wherein said neutralization in step b) is carried out at temperatures in the range of from about 20° C. to about 65° C. and pressures in the range of from about 1 atmosphere to about 2 atmospheres.
Claim 23
Dependent Claim
41 words
The process of claim 12 wherein said saponification in step c) is carried out at a temperature in the range of from about 80° C. to about 105° C. and a pressure of from about 1 atmosphere to about 2 atmospheres.
Claim 24
Dependent Claim
25 words
The process of claim 12 wherein the nonionic organic liquid diluent is selected from the group consisting of aliphatic hydrocarbons, aromatic carbons and mixtures thereof.
Claim 25
Dependent Claim
25 words
The process of claim 22 wherein the nonionic organic liquid diluent is selected from the group consisting of heptane, toluene, isooctane, nonane, and mixtures thereof.
Claim 26
Dependent Claim
16 words
The process of claim 12 wherein the nonionic organic liquid diluent is added in step a).
Claim 27
Dependent Claim
16 words
The process of claim 12 wherein the nonionic organic liquid diluent is added in step b).
Claim 28
Dependent Claim
16 words
The process of claim 12 wherein the nonionic organic liquid diluent is added in step c).
Claim 29
Dependent Claim
35 words
The process of claim 12 wherein said product recovered in step d) contains from about 80 percent by weight to about 99 percent by weight secondary alkyl sulfate, basis the weight of recovered crystallized solid.
Claim 30
Dependent Claim
15 words
The process of claim 12 wherein said glycol in step e) is an alkyl glycol.
Claim 31
Dependent Claim
26 words
The process of claim 28 wherein said alkyl glycol is selected from the group consisting of 1,2-propanediol, diethylene glycol, ethylene glycol, 1,4-butanediol, glycerine and mixtures thereof.
Claim 32
Dependent Claim
47 words
The process of claim 12 wherein said lower phase product in step f) which contains a non-solid secondary alkyl sulfate-containing surface active composition contains from about 5 percent by weight to about 60 percent by weight secondary alkyl sulfate, basis the weight of the lower phase product.
References Cited (Backward Citations)
US2094546A
Cited
US2155027A
Cited
US2640070A
Cited
US2945818A
Cited
GB884656A
Cited
US3234258A
Cited
GB1194862A
Cited
US3681424A
Cited
US3676523A
Cited
US3686351A
Cited
US3893940A
Cited
US3737475A
Cited
US3825615A
Cited
US4088598A
Cited
US4052342A
Cited
US4020121A
Cited
US4226797A
Cited
GB1585030A
Cited
US4322367A
Cited
US4474678A
Cited
US4544493A
Cited
US4857213A
Cited
US5075041A
Cited
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