# US 2019/0314737 A1 · Process for the isolation of levulinic acid

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- Number: US 2019/0314737 A1
- Document ID: US20190314737A1
- Status: Published application
- Kind: A1
- Application number: 16/453,188
- Filed: 2019-06-26
- Published: 2019-10-17
- Earliest claimed: 2015-07-10
- Assignees: Gfbiochemicals IP Assets B.V.
- Applicants: Gfbiochemicals IP Assets B.V.
- Inventors: Aris DE RIJKE; Rudy Francois Maria Jozef PARTON; Donato SANTORO
- Web page: https://patentgrep.com/patent/US20190314737A1

## CPC

- B01D 3/009: {in combination with chemical reactions}
- B01D 1/26: Multiple-effect evaporating
- C07C 51/44: by distillation
- B01D 2257/70: Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- C07C 59/185: Saturated compounds having only one carboxyl group and containing keto groups
- Y02P 20/10: Process efficiency
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

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.

## Claims

### Claim 1

A plant for the production of levulinic acid, comprising: an isolation section formed by a series of three to eight evaporators in series.

### Claim 2 (depends on 1)

The plant according to claim 1, wherein the isolation section is formed by a series of three to six evaporators in series.

### Claim 3 (depends on 1)

The plant according to claim 1, wherein the evaporators are selected from the group of kettle evaporators, internal reboilers, thermo-syphon evaporators, plate and frame heat exchangers, spiral wound heat exchangers, shell and tube heat exchangers, forced circulation evaporators, falling film evaporators, rising film evaporators or agitated thin film evaporators.

### Claim 4 (depends on 1)

The plant according to claim 1, wherein the isolation section comprises at least one agitated thin film evaporator.

### Claim 5 (depends on 4)

The plant according to claim 4, wherein said agitated thin film evaporator is selected from the group of vertical agitated thin film evaporator, horizontal agitated thin film evaporator or a spray dryer; preferably, the agitated thin film evaporator is a vertical agitated thin film evaporator.

### Claim 6 (depends on 1)

The plant according to claim 1, wherein the isolation section comprises at least one forced circulation evaporator and at least an agitated thin film evaporator.

### Claim 7 (depends on 1)

The plant according to claim 1, wherein the isolation section comprises a succession of a forced circulation evaporator, a first agitated thin film evaporator and a second agitated thin film evaporator.

### Claim 8 (depends on 7)

The plant according to claim 7, wherein a first evaporator is a forced circulation evaporator, a second evaporator is a first agitated thin film evaporator and a third evaporator is a second agitated thin film evaporator.

### Claim 9 (depends on 8)

The plant according to claim 8, wherein the first evaporator is operated at a pressure between 5-500 kPa, the second evaporator is operated at a pressure between 1-20 kPa, and the third evaporator is operated at a pressure between 0.1-7.5 kPa.

### Claim 10 (depends on 1)

The plant according to claim 1, wherein the evaporators are operated at a liquid temperature between 100 and 200° C.

### Claim 11 (depends on 1)

The plant according to claim 1, comprising
a pretreatment reactor for mixing C6 carbohydrate-containing feedstock, water and an acid catalyst;
a reactor; wherein in operation the mixture from said pretreatment reactor is fed to the reactor;
a steam feed to said reactor; wherein said steam feed heats and pressurizes the mixture in said reactor;
a flash tank; wherein in operation the mixture from said reactor is fed from said reactor to the said flash tank; wherein said flash tank is at atmospheric pressure.

### Claim 12 (depends on 11)

The plant according to claim 11, further comprising
a neutralization feed to said flash tank, wherein in operation said neutralization feed neutralizes the mixture in said flash tank;
a filtration unit; wherein in operation said filtration unit filters the neutralized mixture thereby removing char from the mixture resulting in a first solution.

### Claim 13 (depends on 12)

The plant according to claim 12, wherein in operation the first solution is fed

### Claim 14 (depends on 12)

The plant according to claim 12, wherein in operation the first solution is fed into a first evaporator thereby removing solvent from the first solution resulting in a second solution; feeding the second solution in a second evaporator thereby removing formic acid from the second solution resulting in a third solution; feeding the third solution in a third evaporator thereby removing tar from the third solution resulting in levulinic acid.
