Gfbiochemicals IP Assets B.v.

Donato Santoro

Rudy Francois Maria Jozef Parton

Aris De Rijke

Barthel Engendahl

De Aris Rijke

A process for the isolation of levulinic acid obtained by acid catalyzed hydrolysis of a C6-carbohydrate-containing feedstock, including the following steps: a) providing a solutioncomprising at least 5 wt. % of levulinic acid, at least 0.1 wt. % of formic acid and at most 94.9 wt. % of solvent, relative to the total weight of solutionb) feeding solutionto a first evaporation step to treat solutionand to obtain solutioncomprising at least 25 wt. % of levulinic acid, less than 20 wt. % of solvent and at least 1 wt. % of formic acid, relative to the total weight of solution, c) feeding solutionto a second evaporation step to treat solutionand to obtain solutioncomprising at least 30 wt. % of levulinic acid and less than 1.0 wt. % of formic acid, relative to the total weight of solutiond) feeding solutionto a third evaporation step to treat solutionand to obtain levulinic acid with a purity of at least 90 wt. % and containing less than 1000 wppm angelica lactone.

Process for the isolation of levulinic acid

A process for the isolation of levulinic acid obtained by acid catalyzed hydrolysis of a C6-carbohydrate-containing feedstock, including the following steps: a) providing a solution 1 comprising at least 5 wt. % of levulinic acid, at least 0.1 wt. % of formic acid and at most 94.9 wt. % of solvent, relative to the total weight of solution 1, b) feeding solution 1 to a first evaporation step to treat solution 1 and to obtain solution 2, comprising at least 25 wt. % of levulinic acid, less than 20 wt. % of solvent and at least 1 wt. % of formic acid, relative to the total weight of solution 2, c) feeding solution 2 to a second evaporation step to treat solution 2 and to obtain solution 3, comprising at least 30 wt. % of levulinic acid and less than 1.0 wt. % of formic acid, relative to the total weight of solution 3, d) feeding solution 3 to a third evaporation step to treat solution 3 and to obtain levulinic acid with a purity of at least 90 wt. % and containing less than 1000 wppm angelica lactone.

A process for the purification of levulinic acid including the following steps: a. providing a composition 1, comprising at least 75 wt. % of levulinic acid; b. cooling composition 1 to at least one temperature Tc, wherein Tc is a temperature in the range 1.23*(W1)&#x2212;104.5&#x2264;Tc (&#xb0; C.)&#x2264;1.23*(W1)&#x2212;89.5, wherein W1 is the weight % of levulinic acid in composition 1, to obtain a cooled composition 1; c. performing melt crystallization of composition 1 including the steps of: i. bringing the cooled composition 1 into contact with levulinic acid crystal seeds, ii. allowing the levulinic acid in composition 1 to crystallize at at least one temperature Tc to obtain crystals 1 and liquid 1, and iii. draining of liquid 1; d. optionally, treating crystals 1, after draining of liquid 1, by sweating, according to the following steps: i. heating the crystals 1 at a temperature between 5 and 40&#xb0; C. to obtain crystals 2 and liquid 2, and ii. draining of liquid 2; e. melting the crystals 1 or 2, after draining of liquid 1 or 2, to obtain composition 2, f. determining the levulinic acid concentration in composition 2 and, in case the levulinic acid concentration is below a predetermined value, repeating steps b, c, optionally d, and e, as many times as necessary to obtain a final composition with a predetermined levulinic acid concentration.

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Valletta, Malta

Donato Santoro