Process for producing furfural

• US 4,912,237 A
• Filed: 01/09/1989
• Issued: 03/27/1990
• Est. Priority Date: 01/08/1988
• Status: Expired due to Fees

• Current Assignee: Fried. Krupp Gesellschaft mit beschrankter Haftung
• Original Assignee: Fried. Krupp Gesellschaft mit beschrankter Haftung
• Inventors: Zeitsch, Karl J.
• Primary Examiner(s): Raymond, Richard L.
• Application Number:
  US07/295,314
• Time in Patent Office: 442 Days
• Field of Search: 549/489
• US Class Current: 549/489
• CPC Class Codes: C07D 307/50 Preparation from natural products

Abstract

A feed suspension of pentosan-containing organic raw materials in dilute sulfuric acid is passed with low residence time through a flow reactor heated by high-pressure steam to 170°-230° C. and then through a cooler in which it is cooled to 140°-200° C. before the suspension is admitted to a flash evaporating unit from which a furfural-rich vapor phase is separated from the residual suspension. Process water is recovered from the residual suspension and recycled for the preparation of the feed suspension. From the vapor phase, furfural is recovered by distillation, either directly or after liquefaction. In the latter case, partial condensation in a primary condenser can be used to increase the furfural concentration in the final condenser, the condensate of the primary condenser being recycled for the preparation of the feed suspension.

Claims

1. A process for making furfural, comprising the steps of:

(a) passing a suspension of a comminuted pentosan-containing raw material in dilute sulfuric acid continuously through a flow reactor and mixing said suspension in said reactor with high-pressure steam to heat said suspension to a temperature between 170° and

230°

C. for a residence time sufficient to hydrolyze and dehydrate pentosan in said raw material to furfural, thereby forming a reacted suspension containing furfural which is discharged from said flow reactor;

(b) cooling the reacted suspension discharged from said reactor in a heat exchanger to a temperature between 140° and

200°

C.;

(c) thereafter passing the reacted suspension, cooled in said heat exchanger, through a valve into an expansion evaporator maintained at a pressure of at most 760 Torr to separate a residual suspension phase containing furfural from a water/furfural mixed vapor phase; and

(d) recovering furfural from the vapor phase by distillation, either directly or after liquefaction.

2. The process defined in claim 1 wherein:

the temperature to which the suspension is heated in said flow reactor is 210°

to 230°

C.; and

said pressure is between 50 and 200 Torr.

3. The process defined in claim 1 wherein, in step (d) said water/furfural mixed vapor phase is subjected to condensation in a first condensing stage to yield a furfural-containing condensate and a vapor having a higher furfural content, and said vapor having said higher furfural content is then condensed in a second condensing stage, said condensate being fed to said reactor in step (a).

4. The process defined in claim 1 wherein said residual suspension phase is dewatered to form an acid and furfural containing process water, said process water being fed to said reactor in step (a).

5. The process defined in claim 1 wherein said residual suspension phase is fed to a filter at which a solid is separated from a filtrate, said solid being initially subjected to extraction of moisture and then washed with water, a liquid recovered by the moisture extraction and a liquid formed by evaporative concentration of the wash water being then utilized to form a mash of fresh quantities of said raw material, vapors of the evaporative concentration being then processed for recovery of furfural therefrom.

6. The process defined in claim 5 wherein said vapors of the evaporative concentration are combined with said water/furfural mixed vapor phase for recovery of furfural therefrom.

7. The process defined in claim 4 wherein a part of said process water is subjected to distillation prior to being fed to the reactor in step (a).

8. The process defined in claim 7 wherein said part is a maximum of 10% of said process water.