Progressing batch hydrolysis process

• US 4,615,742 A
• Filed: 01/10/1985
• Issued: 10/07/1986
• Est. Priority Date: 01/10/1985
• Status: Expired due to Term

• Current Assignee: The United States of America As Represented By The Secretary of Agriculture
• Original Assignee: United States Of America As Represented By The Department Of Energy
• Inventors: Wright, John D.
• Primary Examiner(s): Fisher, Richard V.
• Assistant Examiner(s): Jones, W. Gary
• Application Number:
  US06/690,544
• Time in Patent Office: 635 Days
• Field of Search: 127/1, 127/36, 127/37, 127/42, 162/14, 162/16
• US Class Current: 127/37
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32

Abstract

A progressive batch hydrolysis process for producing sugar from a lignocellulosic feedstock, comprising passing a stream of dilute acid serially through a plurality of percolation hydrolysis reactors charged with said feedstock, at a flow rate, temperature and pressure sufficient to substantially convert all the cellulose component of the feedstock to glucose; cooling said dilute acid stream containing glucose, after exiting the last percolation hydrolysis reactor, then feeding said dilute acid stream serially through a plurality of prehydrolysis percolation reactors, charged with said feedstock, at a flow rate, temperature and pressure sufficient to substantially convert all the hemicellulose component of said feedstock to glucose; and cooling the dilute acid stream containing glucose after it exits the last prehydrolysis reactor.

Claims

1. A progressive batch prehydrolysis and hydrolysis process for producing sugar from a lignocellulosic feedstock, comprising:

(a) providing at least one percolation reactor, said reactor being initially charged with lignocellulosic feedstock including hemicellulose components and cellulose components, which feedstock has not been prehydrolyzed;

(b) prehydrolyzing said feedstock by passing a liquid stream of dilute acid into and then serially through said reactors in (a) which are charged with said lignocellulosic feedstock, said dilute acid being at a temperature, pressure, and flow rate sufficient to convert, by hydrolysis, substantially all of the hemicellulose components of said feedstock to sugar comprising xylose, glucose and other sugars carried by said liquid acid stream without completely hydrolyzing said cellulose components of said feedstock, said liquid stream of dilute acid being at a temperature and maintained at a temperature such that said sugars produced within said reactors from said hemicellulose component and carried by said dilute acid stream are not subjected to any significant heat degradation;

(c) cooling and recovering said dilute sugar containing acid stream after it exits the last reactor in (a);

(d) providing at least one additional percolation reactor initially charged with said lignocellulosic feedstock including hemicellulose components and cellulose components, which feedstock has not been prehydrolyzed;

(e) serially connecting said reactors in (a) to and upstream of said additional reactors in (d);

(f) passing a liquid stream of dilute acid serially through said reactors in (a) which are now charged with prehydrolyzed lignocellulosic feedstock which is now substantially free of unreacted hemicellulose, said liquid stream of dilute acid being at a temperature, said temperature being higher than the temperature of said liquid acid stream in (b), pressure and flow rate sufficient to convert substantially all of said remaining cellulose components of said feedstock to sugars comprising glucose and other sugars carried by said dilute acid stream;

(g) cooling said dilute acid stream containing sugar after exiting the last reactor in (f), and then prehydrolyzing the feedstock in the additional reactors in (d) by feeding said dilute acid stream containing sugar serially through said additional reactors in (d) charged with said lignocellulosic feedstock including hemicellulose components and cellulose components, said dilute acid being at a temperature, pressure and flow rate sufficient to convert by hydrolysis substantially all of the hemicellulose components of said feedstock to sugars comprising xylose, glucose and other sugars carried by said liquid acid stream without completely hydrolyzing said cellulose components of said feedstock, said cooled liquid stream being at a temperature and maintained at a temperature such that said sugars produced from said hemicellulose components of said feedstock are not subjected to any significant heat degradation; and

then

(h) cooling and recovering said dilute sugar containing acid stream after it exits the last reactor in (g).

2. The process of claim 1, wherein said lignocellulosic feedstock comprises wood particles selected from the group consisting of wood chips, sawdust, wood shavings, agricultural residues, municiple solid waste, and mixtures thereof.

3. The process of claim 2, wherein said lignocellulosic feedstock comprises wood chips.

4. The process of claim 1, wherein after the feedstock contained in the first percolation reactor in (f) has been substantially converted to glucose, said reactor is disconnected from the operating sequence, and the supply stream of dilute acid is diverted to the next percolation reactor in the operation.

5. The process of claim 4, wherein a freshly charged percolation reactor is connected as the last additional reactor in the reactors in (d).

6. The process of claim 5, wherein said freshly charged percolation reactor, prior to being serially connected to the process, is exposed to a stream of low pressure steam for a time sufficient to displace the air contained in the feedstock.

7. The process of claim 6, wherein the feedstock in the freshly charged percolation reactor is contacted with dilute acid for a time sufficient to fully soak said feed stock.

8. The process of claim 1, wherein the percolation reactors in (f) are operated at temperatures of about 180°

C. to 190°

C., and the percolation reactors in (b) and (g) are operated at temperatures of about 140°

C. to 150°

C.

9. The process of claim 1, wherein the dilute acid is an inorganic acid selected from the group consisting of sulfuric, hydrochloric, phosphoric, nitric and hydrofluoric.

10. The process of claim 1, wherein the dilute acid is sulfuric.

11. The process of claim 10, wherein the sulfuric acid has a concentration of about 0.2 to about 2 percent.

12. The process of claim 1, wherein the flow rate of the dilute acid stream through the hydrolysis reactors in each batch sequence is adjusted so that the average contact time of the dilute acid with the feedstock contained in the reactor vessels is about 10 to 60 minutes per reactor.

13. The process of claim 12, wherein the average contact time varies from about 15 to 30 minutes per reactor.

14. The process of claim 1, wherein the cooling of the sugar-containing dilute acid stream exiting the last percolation reactors in (f) is accomplished by passing said acid stream through either a flash tank or heat exchanger prior to entering the reactors in (g).

15. The process of claim 1, wherein the cooling of the sugar-containing dilute acid stream exiting the last percolation reactor in (b) and (g) is accomplished by passing said sugar-containing dilute acid stream through a flash tank prior to recovering the sugar-containing acid.

16. The process of claim 1, wherein the temperature profile in the hydrolysis is adjusted by heat exchangers between the hydrolysis percolation reactors.

17. The process of claim 1 wherein the percolation reactors in (f) are operated at temperatures in the range of about 170°

C. to about 200°

C., and the percolation reactors in (b) and (g) are operated at temperatures in the range of about 135°

C. to about 160°

C.

18. A progressive batch prehydrolysis and hydrolysis process for producing sugar from a lignocellulosic feedstock, comprising:

(a) providing at least one percolation reactor, said reactor being initially charged with lignocellulosic feedstock including wood chips having hemicellulose components and cellulose components, which feedstock has not been prehydrolyzed;

(b) prehydrolyzing said feedstock by passing a liquid stream of dilute sulfuric acid having a concentration in the range of about 0.2% to about 2.0% by weight, serially through said reactors in (a) which are charged with said lignocellulosic feedstock, said dilute acid being at a temperature in the range of about 140°

C. to about 150°

C., pressure, and flow rate sufficient to convert, by hydrolysis, substantially all of the hemicellulose components of said feedstock to sugars comprising xylose, gluose and other sugars carried by said liquid sulfuric acid stream without completely hydrolyzing said cellulose components of said feedstock, said liquid stream of dilute acid being at a temperature and maintained at a temperature less than about 160°

C. so that said sugars produced within said reactors from said hemicellulose component and carried by said dilute sulfuric acid stream are not subjected to any significant heat degradation;

(c) cooling and recovering said dilute sugar containing sulfuric acid stream after it exits the last reactor in (a);

(d) providing at least one additional percolation reactor initially charged with said lignocellulosic feedstock including hemicellulose components and cellulose components, which feedstock has not been prehydrolyzed;

(e) serially connecting said reactors in (a) to and upstream of said additional reactors in (d);

(f) passing a liquid stream of dilute sulfuric acid serially through said reactors in (a) which are now charged with prehydrolyzed lignocellulosic feedstock which is now substantially free of unreacted hemicellulose, said liquid stream of dilute sulfuric acid being at a temperature, in the range of about 180°

C. to about 190°

C., pressure and flow rate sufficient to convert substantially all of said remaining cellulose components of said feedstock to sugars comprising glucose and other sugars carried by said dilute acid stream;

(g) cooling said dilute sulfuric acid stream containing sugar after exiting the last reactor in (f), and then prehydrolyzing the feedstock in the additional reactors in (d) by feeding said dilute sulfuric acid stream containing sugar serially through said reactors in (d) charged with said lignocellulosic feedstock including hemicellulose components and cellulose components at a temperature in the range of about 140°

C. to about 150°

C., pressure and flow rate sufficient to convert by hydrolysis substantially all of the hemicellulose components of said feedstock to sugars comprising xylose, glucose and other sugars carried by said liquid acid stream without completely hydrolyzing said cellulose components of said feedstock, said cooled liquid stream being at a temperature and maintained at a temperature less than about 160°

C. so that said sugars produced from said hemicellulose components of said feedstock are not subjected to any significant heat degradation; and

then

(h) cooling and recovering said dilute sugar containing sulfuric acid stream after it exits the last reactor in (g).