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Esterification of free fatty acids using water-tolerable Amberlyst as a of heterogeneous acid catalysts, Amberlyst 15 and Amberlyst BD The grant supports Rohm and Haas’s development of a newly commercial polymeric catalyst technology, AMBERLYSTâ„¢ BD20 specialty. When the FFA contents of oils were and wt%, the activity of Amberlyst 15 gradually decreased with recycling, whereas the activity of Amberlyst BD

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Esterification of free fatty acids using water-tolerable Amberlyst as a heterogeneous catalyst.

Method for producing alkyl carboxylates by multi-stage esteridication interrupted with a dehydration step. The calculated molar ratio of methanol to free fatty acid was 9. In another embodiment method is repeated one or more times in series or parallel with method The final reaction mixture has reduced free fatty acids compared to the feedstock entering and to the reaction mixture leaving the first reactor. In one embodiment it may be beneficial to minimize the amount of homogenous catalyst in stream Depending on the unit operation desired, unit may operate at temperatures and pressures above or below atmospheric conditions.

After a prescribed residence time and set of operating conditions the second reaction mixture exits the reactor with reduced free ambeglyst acids and enters a separation stage.

In a vertical amberlysf, the reactants may flow upwards or downwards through the reactor In any embodiment, dry reaction mixture 9 proceeds to a second reactor which may or may not contain heterogeneous catalyst. Pressure is generally maintained at a constant level throughout the reaction.

Furthermore, regeneration or catalyst replacement is a time-consuming and waste-generating activity which puts normal plant production on hold and adds costs for waste disposal. Purification of glycerin obtained as a bioproduct from the transesterification of triglycerides in the synthesis of biofuel.

The methods of the invention can accommodate a wide range of feedstocks. This application is based upon U. Some variations of the present invention consist of a method of esterification using a dual catalyst process that produces a product stream with sufficiently low FFA in which the amount of FFA in the product stream leaving the process remains stable over time.

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This process reduces the overall yield of feedstock to FAAE though and generates a stream amberlysy concentrated FFA that requires finding a new end-use, further processing or disposal.

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For a variety of feedstocks and experimental conditions increasing product FFA trends have been observed with Amberlyst ion exchange resin catalyst supporting the catalyst deactivation theory. However, additional reaction stages require capital investment for additional unit operations as well as additional operating expenses. The second reaction mixture 10 enters unit which may be a decanter, centrifuge, flash evaporator, flash drum, vacuum distillation column or other separation unit.

Process amberlyts extraction and catalytic esterification of fatty acids found in sewage scum. Another pretreatment process used to convert FFA into esters is acid catalyzed esterification.

One or more guard beds may be employed in series or parallel.

Esterification of free fatty acids using water-tolerable Amberlyst as a heterogeneous catalyst.

In one embodiment, method in FIG. The method of claim 13wherein the reactor is a continuous flow reactor.

In one embodiment the regenerating acid flow in the opposite direction countercurrent of the service flow, noting the service flow may be upwards or downwards through the reactor. The method of claim 1further comprising the step of separating a majority of the alcohol and water from the reaction mixture to obtain a dry reaction mixture. The method of claim 1wherein the combination of said homogeneous catalyst and said heterogeneous catalyst provide increased conversion relative to the use of either catalyst alone.

The method of claim 1wherein the feedstock, alcohol, and homogeneous catalyst flow upward through said reactor. In one embodiment, the reaction time in unit is around minutes, and in another embodiment the reaction time is around minutes. Therefore, in one embodiment of this invention, the final FFA content of the reaction mixture leaving the process during steady state operation bf20 stable over time, that is, the final FFA content does not consecutively increase or decrease so as to create a trend.


The reactor contains a predetermined amount of heterogeneous catalyst. What is needed in the art are methods that improve upon the respective challenges and disadvantages posed by homogenous and heterogeneous catalyst use for esterification of carboxylic acids.

The invention is illustrated in detail below with reference to the examples, but without restricting it to them. In any embodiment, dry reaction mixture 12 may continue to a transesterification, hydrogenation or other catalytic chemical conversion process, alcohol may ambeelyst recovered from stream 11 and a portion of homogenous catalyst may be recovered from either stream 11 or In another embodiment, the Amberlyt is selected between 0.

In one embodiment the pressure is maintained between 0 and psig. Heterogeneous catalysis often provides good selectivity and, unlike most homogeneous catalysts, are designed to be used for extended periods of time, which avoids the continuous operating expense of unrecoverable homogeneous catalysts. In one embodiment, the final reaction mixture 35or 10 is separated into an alcohol and water phase and an oil phase also referred to herein as the dry reaction mixture.

FFA testing of the dry reaction mixture was completed as described in Example 1 except that a double water wash was performed to remove all MSA. Year of fee payment: A continuous process for the preparation of esters of aliphatic carboxylic acids.

Another common method to remove small amounts of FFA is by adding a base reactant such as sodium hydroxide in order to saponify the FFA to soap which allows removal by water washing and filtration.

However, there are unresolved concerns about catalyst fouling, durability, stability, activity, and replacement schedule with continuous use of commercial-grade higher FFA feedstocks.

In another embodiment, a portion of alcohol, water and homogenous catalyst 8 are removed from the first reaction mixture 3 contained in unit by decantation or centrifugation, leaving a principally dry reaction mixture 9.