Method of producing level off DP microcrystallinecellulose and glucose from lignocellulosic material

• US 4,645,541 A
• Filed: 12/04/1985
• Issued: 02/24/1987
• Est. Priority Date: 08/02/1984
• Status: Expired due to Fees

• Current Assignee: Tigney Technology Incorporated
• Original Assignee: Edward A. Delong
• Inventors: DeLong, Edward A.
• Primary Examiner(s): NOT, DEFINED
• Assistant Examiner(s): Pak, Chung K.
• Application Number:
  US06/804,547
• Time in Patent Office: 447 Days
• Field of Search: 127/37, 127/1, 162/14, 162/16, 162/9, 162/21, 162/22, 162/28, 162/247, 536/56, 435/101, 435/165, 435/105, 435/277, 435/278, 426/53, 426/52, 426/573, 426/658
• US Class Current: 127/37
• CPC Class Codes: C08B 15/02 Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32

Abstract

Microcrystalline cellulose has many applications in the pharmaceutical, food, paper and structural composite industries. Level off DP (Degree of Polymerization) microcrystalline cellulose is made up of a chain of about 250 glucose molecules in the form of microcrystal. In nature, several microcrystals are hinged together and surrounded by amorphous cellulose to form a cellulose microfibril. If the amorphous cellulose is removed, the resultant product is called level off DP (Degree of Polymerization) microcrystalline cellulose. When lignocellulosic material is processed according to applicant'"'"'s earlier processes (Canadian Pat. Nos. 1,096,374 and 1,141,376), the dissociated material is partitioned by removing the lignin and the xylan leaving a low DP (320) cellulose fraction. This material can be converted to level off DP microcrystalline cellulose and glucose by soaking the cellulose in an acid solution, dewatering it, returning the acid-impregnated cellulose to the reactor, introducing high pressure steam (300-700 psi) and when substantially all of the material reaches a temperature of the order of 215° C., releasing it instantly to atmosphere. This procedure will produce a mixture of level off DP microcrystalline cellulose and glucose. If the acid solution employed is sulfuric acid and the temperature of the cellulose is allowed to reach a uniform temperature of 234° C. before instant release to atmosphere, the procedure will produce substantially all glucose.

Claims

1. A method of producing level off DP microcrystalline cellulose and glucose from lignocellulosic material, comprising:

(a) packing the lignocellulosic material in a divided, exposed, moist form in a pressure vessel having a valved outlet,

(b) with the valved outlet closed, rapidly filling the pressure vessel with steam at a pressure of 400-700 psi to bring, by means of the pressurized steam, substantially all of the lignocellulosic material to a temperature in the range 185°

to 240°

C. in less than 60 seconds to thermally soften the lignocellulosic material into a plastic condition, and

(c) as soon as the said plastic condition has been attained, opening the valved outlet and explosively expelling the lignocellulosic material in the said plastic condition, from the pressure vessel through the outlet to atmosphere so that the said material issues from the outlet in particulate form with lignin therein rendered into particles substantially in the range 1 to 10 microns and separable from the cellulose and hemicellulose, the particulate lignin, hemicellulose and cellulose being together in dissociated form having the appearance of potting soil, a major portion of the lignin being soluble in methanol or ethanol and being thermoplastic, the cellulose being in the form of crystalline alpha cellulose microfibrils and suitable for digestion or conversion by micro-organisms and enzymes,

(d) separating the cellulose in the particulate material from the lignin and hemicellulose,

(e) soaking the separated cellulose in an acid solution of at least one acid selected from the group consisting of sulfuric acid, hydrochloric acid and sulfurous acid until the acid is distributed evenly throughout the cellulose, and then reducing the moisture content of the cellulose, leaving the cellulose impregnated with acid at a concentration in the range 0.05% to 2.0% of the weight of the cellulose,

(f) packing the acid-impregnated cellulose into a pressure vessel having a valved outlet,

(g) rapidly filling the pressure vesel with steam to a pressure in the range 300 psi to 700 psi to bring, by means of the pressurized steam, substantially all of the acid-impregnated cellulose to a temperature in the range of 185°

-240°

C. in less than 60 seconds, and thereby weaken by hydrolysis and thermal softening, the intramolecular bonds joining the glucose units to form the cellulose, then

(h) opening the valved outlet, and explosively expelling the acid-impregnated cellulose from the pressure vessel through the outlet to atmospheric pressure, thereby breaking the intramolecular cross-links in the cellulose to depolymerize the hydrolysed, acid-impregnated cellulose to produce a mixture of cellulose and a glucose solution therefrom, and thereby rapidly reducing the temperature of the extruded material to below 100°

C. to prevent further depolymerization of the cellulose and degradation of the glucose, and then

(i) neutralizing the acidity of the glucose solution and residual cellulose.

2. A method according to claim 1, wherein any residual cellulose is filtered from the glucose solution.

3. A method according to claim 1, wherein the acid-impregnated cellulose is reduced to a moisture content of the level in the range of 20% to 80% by weight of the cellulose before being packed into the pressure vessel.

4. A method according to claim 1, wherein the end product is a mixture of glucose from the amorphous component of the cellulose and level off DP microcrystalline cellulose from the crystalline alpha cellulose fraction of the cellulose, and the cellulose is impregnated with acid at a concentration of 0.05% to 1.0% of the weight of the cellulose, and the pressure vessel is rapidly filled with steam to a pressure between 350 psi and 550 psi to bring the acid-impregnated cellulose to a temperature in the range of 200°

C. to 225°

C. in less than 60 seconds.

5. A method according to claim 1, wherein the end product is a mixture of glucose from the amorphous component of the cellulose and level off DP microcrystalline alpha cellulose from the crystalline alpha cellulose fraction of the cellulose, and the cellulose is impregnated with hydrochloric acid at a concentration of about 0.2% of the weight of the cellulose, and the pressure vessel is rapidly filled with steam to a pressure of about 450 psi to bring the acid-impregnated cellulose to a temperature of about 215°

C. in less than 45 seconds.

6. A method according to claim 1, wherein the end product is substantially all glucose, the pressure vessel is rapidly filled with steam to a pressure in the range 400 psi to 700 psi, to bring the cellulose, which has been impregnated with sulfuric acid to a level in the range 0.5% to 1.5% of the weight of the cellulose, to a temperature in the range 215°

C. to 240°

C., in less than 60 seconds.

7. A method according to claim 1, wherein the end product is substantially all glucose, the pressure vessel is rapidly filled with steam to a pressure of about 650 psi to bring the cellulose, which has been impregnated with sulfuric acid to a level of about 1% of the weight of the cellulose, to a temperature of about 234°

C., in less than 45 seconds.

8. A method according to claim 1, wherein liquid condensate is removed from the bottom of the pressure vessel as it is formed.

9. A method according to claim 1, wherein steps (e) to (i) are repeated on any residual cellulose.

10. A method according to claim 1, wherein any residual cellulose is treated with enzymes for the conversion thereof to glucose.