Process for the continuous production of lower alkyl esters of higher fatty acids
First Claim
1. In a process for the continuous production of lower alkyl esters of higher fatty acids wherein lower alcohol and an oil phase of fatty triglycerides or natural oils or fats containing free fatty acids is subjected to catalytic transesterification at reaction temperatures of up to 100°
- C. in the presence of an alkaline catalyst, and glycerine, catalyst residue alcohol reactant are removed, the improvement which comprises, in sequence,a) introducing a reaction mixture which is pre-mixed combination of oil phase, alcohol and catalyst at reaction temperature into the top of a reactor column such that the rate of flow is less than the sinking rate of the glycerine which separates from the reaction mixture and separating free glycerine from the column transesterification product,b) transferring the column transesterification product which contains dissolved and dispersed glycerine, lower alkyl esters, alcohol, catalyst, oil and partially transformed oil, to a second reactor which is at reaction temperatures and conducting a further transesterification,c) washing the thus obtained reaction mixture with an aqueous extractant in a first separator,d) introducing the thus washed reaction mixture, additional alcohol and catalyst into a third reactor at reaction temperature and at a flow speed conforming to the stage a) of the process,e) introducing the resulting mixture into a fourth reactor and maintaining the mixture under stirring for a further transesterification, forming a reaction product have a degree of transesterification of at least 99.2%,f) introducing the resulting transesterification product and hot, aqueous extractant solution into a second separator and separating alcohol, glycerine, soaps formed and catalyst from the transesterification product, andg) drying the transesterification product.
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Abstract
Production of lower alkyl esters of higher fatty acids from an oil phase and lower alcohols by catalytic transesterification at reaction temperatures of up to 100° C. in the presence of an alkaline catalyst, includes a) introducing a mixture of oil phase, alcohol and catalyst at reaction temperature into the top of a first reactor column, at a rate of flow which is lower than the sinking rate of the glycerine separated from the reaction mixture, b) the reaction mixture is passed into a second reactor for further transesterification, c) the thus obtained reaction mixture is further freed of glycerine in an initial separating stage by means of a short-term washing, d) the reaction mixture is passed into a third reactor with addition of further alcohol and catalyst, and at a rate of flow conforming to the first stage of the process, e) the reaction mixture is further transesterified, f) reaction product is freed of the remaining methanol, glycerine, soaps formed and catalyst in a second separating stage, under addition of an aqueous extraction buffer solution, and g) the reaction mixture is freed of lower alcohols by stripping, washed with suitable extraction and washing solutions and dried.
152 Citations
16 Claims
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1. In a process for the continuous production of lower alkyl esters of higher fatty acids wherein lower alcohol and an oil phase of fatty triglycerides or natural oils or fats containing free fatty acids is subjected to catalytic transesterification at reaction temperatures of up to 100°
- C. in the presence of an alkaline catalyst, and glycerine, catalyst residue alcohol reactant are removed, the improvement which comprises, in sequence,
a) introducing a reaction mixture which is pre-mixed combination of oil phase, alcohol and catalyst at reaction temperature into the top of a reactor column such that the rate of flow is less than the sinking rate of the glycerine which separates from the reaction mixture and separating free glycerine from the column transesterification product, b) transferring the column transesterification product which contains dissolved and dispersed glycerine, lower alkyl esters, alcohol, catalyst, oil and partially transformed oil, to a second reactor which is at reaction temperatures and conducting a further transesterification, c) washing the thus obtained reaction mixture with an aqueous extractant in a first separator, d) introducing the thus washed reaction mixture, additional alcohol and catalyst into a third reactor at reaction temperature and at a flow speed conforming to the stage a) of the process, e) introducing the resulting mixture into a fourth reactor and maintaining the mixture under stirring for a further transesterification, forming a reaction product have a degree of transesterification of at least 99.2%, f) introducing the resulting transesterification product and hot, aqueous extractant solution into a second separator and separating alcohol, glycerine, soaps formed and catalyst from the transesterification product, and g) drying the transesterification product. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16)
- C. in the presence of an alkaline catalyst, and glycerine, catalyst residue alcohol reactant are removed, the improvement which comprises, in sequence,
Specification
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- Resources
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Current AssigneeOelmuhle Leer Connemann GmbH & Co.
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Original AssigneeOelmuhle Leer Connemann GmbH & Co.
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InventorsKrallmann, Anton, Fischer, Erich, Connemann, Joosten
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Primary Examiner(s)Dees, Jose G.
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Assistant Examiner(s)Jones, Dwayne C.
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Application NumberUS08/037,224Time in Patent Office564 DaysField of Search554/168, 554/167US Class Current554/167CPC Class CodesC07C 67/03 by reacting an ester group ...C07C 69/24 esterified with monohydroxy...C07C 69/52 Esters of acyclic unsaturat...
