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, AMBERLYST™ 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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The reaction is conducted using at least a stoichiometric amount of bc20 as determined on an FFA basis according to Equation 1. However, additional reaction stages require capital investment for additional unit operations as well as additional operating expenses. Another method of the invention, with reference to FIG. The method of claim 2wherein said carboxylic acids are free fatty acids. The calculated molar ratio of methanol to free fatty acid was 9.

The method of claim 25further comprising the zmberlyst of processing the second reaction mixture in one of a transesterification process and a hydrotreating process. Depending on the unit operation desired, unit may operate at temperatures and pressures above or below atmospheric conditions. In one embodiment the feedstock containing carboxylic acid is pretreated to remove excess water and impurities.

However, there are unresolved concerns about catalyst fouling, durability, stability, activity, and replacement schedule with continuous use of commercial-grade higher FFA feedstocks. In one embodiment the first reaction mixture 3 is washed with water before entering a decanter The method of claim 13wherein the dry reaction mixture bd2 a principally dry reaction mixture.

AMBERLYST™ BD20 – KDY Holdings

The total contact time of feedstock and methanol with MSA was approximately 70 minutes. The second reaction mixture 5 enters unit which may be a decanter, centrifuge, flash evaporator, flash drum, vacuum distillation column, or other similar separation unit.

One or amberlyt guard beds may be employed in series or parallel. What is claimed is: The invention converts free fatty acids into esters by esterification with alcohol and a dual catalyst such that the reaction mixture contains sufficiently low free fatty acids and the amount of free fatty acids in the product stream leaving the process remains stable over time. Simultaneous synthesis and purification of a fatty acid monoester biodiesel fuel. Homogenous catalysis provides excellent selectivity and activity.


The regeneration may be performed in multiple steps with different acid concentrations and residence times in each step.

In another embodiment, the residence time is between 5 and minutes. The first reaction mixture 3 enters unit which may be a decanter, centrifuge, flash ambeglyst, vacuum distillation column or other separation unit.

US8957242B2 – Dual catalyst esterification – Google Patents

It may be a continuously-stirred tank, plug-flow, tubular-flow, mixed-flow, fixed bed, fluidized bed, batch, semi-batch, recirculating, or other reactor type. Such contaminants bd02 be introduced by the feedstock, corrosion, and other akberlyst or mechanism within the process. The FFA esterification reaction is affected by temperature, molar ratio of alcohol to FFA, mass transfer limitations, catalyst concentration, reaction time, and reaction stoichiometry. US USA1 en However, adding the homogenous catalyst to the feedstock before the reaction mixture reaches the heterogeneous catalyst or into the heterogeneous catalyst reactor: Comparing Example 1 and 2 amberlywt is clear the added MSA has two effects: In any embodiment it may be preferable to minimize the amount of moisture in stream 7.

The method of claim 1wherein the feedstock, alcohol, and homogeneous catalyst flow upward through said reactor.

The residence time of the acid though amberlysh catalyst bed should be approximately minutes. 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.

The homogenous catalyst may be contained in either or both phases. One method of the invention, with reference to FIG. The final average FFA content of the dry reaction mixture was 0. In some situations the pressure may be below the vapor pressure of the alcohol although the alcohol may reflux back into the reaction mixture.

In one embodiment, unit may have operating conditions and provisions as previously described for unit when charged with heterogeneous catalyst; whereas unit may have operating conditions and provisions as described for unit when not containing heterogeneous catalyst. The method of claim 22further comprising amverlyst step of reacting the second stream in a second reactor with at least one of additional homogeneous catalyst, additional heterogeneous catalyst, and additional alcohol to form a second reaction mixture.


The reactor may have freeboard space above the catalyst bed to allow for catalyst movement and expansion as known to amherlyst skilled in the art.

This process reduces the overall amberlysy of feedstock to FAAE though and generates a amberlyat of concentrated FFA that requires finding a new end-use, further processing or disposal. In one embodiment, the alcohol described in the invention is dry methanol. Additionally, feedstocks may include bf20 or distilled fats and oils including fatty acid distillates, palm fatty acid distillate, and others. The second reaction mixture 10 enters aamberlyst which may be a decanter, centrifuge, flash evaporator, flash drum, vacuum distillation column or other separation unit.

In one embodiment the regenerating acid flow in the opposite direction countercurrent of the service flow, noting the service amberlgst may be upwards or downwards through the reactor. In any embodiment, dry reaction mixture 7 may continue to a transesterification process, alcohol may be recovered from stream 6 and a portion of homogenous catalyst may be recovered from either stream 6 or 7.

In one embodiment, alcohol 2 is introduced to a feedstock containing carboxylic acid 1 and homogenous catalyst.

Approximately g of feedstock was fed over 6. A dual catalyst process can also reduce the continuous operating expense of using unrecoverable homogeneous catalysts by reducing the amount of homogeneous catalyst required to obtain the advantages of homogeneous catalyst use. Purification of glycerin obtained as a bioproduct from the transesterification of triglycerides in the synthesis of biofuel.