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US3970712A Expired / Lapsed US ⏱️ 0.0 years remaining

Hydrolysis of oat husks

Assignee: Sued Chemie AG
•
Filing: 1974-11-13
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Granted: 1976-07-20
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Expires: 1994-11-13
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Abstract

Abstract A process for the hydrolysis of oat husks is carried out with alkali metal hydroxide or alkali metal chlorite in a first stage and with mineral acid in a second stage to provide D-(+)-xylose. The xylose can be recovered as such, or converted in situ to xylitol. The solid residue by-product of the aforesaid process for the hydrolysis of oat husks, following removal of the lignin content thereof, is readily convertible to cellulose.

Inventors

  • 👤 Hermann Friese

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-07 21:23
CPC Classifications
D; D21; D21C; D21C5/00; C; C13; C13K; C13K13/00; C13K13/002

Claims Analysis

Total Claims: 32
Claim 1
Independent Claim 102 words
A process for the hydrolysis of oat husks which comprises: a. hydrolyzing oat husks with a solvent containing at least one member selected from the group consisting of alkali metal hydroxide and alkali metal chlorite to provide oat husks from which the chemically bound acetic acid originally present therein has been substantially completely removed, and a solution of acetic acid; b. recovering the oat husks from which the chemically bound acetic acid has been substantially removed; and c. hydrolyzing the oat husks of step (b) with a mineral acid to provide a solid residue containing lignin and an acidic solution of D-(+)-xylose.
Claim 2
Dependent Claim 102 words
A process for the hydrolysis of oat husks which comprises: a. hydrolyzing oat husks with a solvent containing at least one member selected from the group consisting of alkali metal hydroxide and alkali metal chlorite to provide oat husks from which the chemically bound acetic acid originally present therein has been substantially completely removed, and a solution of acetic acid; b. recovering the oat husks from which the chemically bound acetic acid has been substantially removed; and c. hydrolyzing the oat husks of step (b) with a mineral acid to provide a solid residue containing lignin and an acidic solution of D-(+)-xylose.
Claim 3
Dependent Claim 57 words
The process of claim 1 wherein the solid residue containing lignin is separated from the acidic solution of D-(+)-xylose, the residue is extracted with organic solvent to remove the lignin therefrom and the remaining residue is treated with at least one member of the group consisting of alkali metal chlorite and alkali metal hydroxide at elevated temperature.
Claim 4
Dependent Claim 23 words
The process of claim 1 wherein the D-(+)-xylose present in the acid solution of step (c) is recovered therefrom in substantially pure form.
Claim 5
Dependent Claim 36 words
The process of claim 1 wherein the acid employed in hydrolysis step (c) is sulphuric acid, the acidic solution of D-(+)-xylose is neutralized with base and the xylose is thereafter reduced in situ to provide xylitol.
Claim 6
Dependent Claim 16 words
The process of claim 4 wherein the xylitol is recovered from solution in substantially pure form.
Claim 7
Dependent Claim 19 words
The process of claim 2 wherein the lignin is recovered from the extract solution thereof in substantially pure form.
Claim 8
Dependent Claim 23 words
The process of claim 1 wherein hydrolysis step (a) is carried out with a solution of sodium hydroxide, potassium hydroxide or combination thereof.
Claim 9
Dependent Claim 12 words
The process of claim 7 wherein the solution is an aqueous solution.
Claim 10
Dependent Claim 34 words
The process of claim 7 wherein hydrolysis step (a) is carried out under ambient pressure with an alkali metal hydroxide concentration of 0.6 to 4% by weight based on solvent and alkali metal hydroxide.
Claim 11
Dependent Claim 24 words
The process of claim 9 wherein the alkali metal hydroxide concentration is 1 to 2% by weight based on solvent and alkali metal hydroxide.
Claim 12
Dependent Claim 18 words
The process of claim 9 wherein a temperature of 15° to 100°C. is employed in hydrolysis step (a).
Claim 13
Dependent Claim 18 words
The process of claim 11 wherein a temperature of 20° to 60°C. is employed in hydrolysis step (a).
Claim 14
Dependent Claim 35 words
The process of claim 7 wherein hydrolysis step (a) is carried out under elevated pressure with an alkali metal hydroxide concentration of 0.3 to 1.5 % by weight based on alkali metal hydroxide and solvent.
Claim 15
Dependent Claim 24 words
The process of claim 13 wherein the alkali metal hydroxide concentration is 0.5 to 1% by weight based on solvent and alkali metal hydroxide.
Claim 16
Dependent Claim 27 words
The process of claim 13 wherein hydrolysis step (a) is carried out at a pressure up to 3 atmospheres gauge and at a temperature up to 125°C.
Claim 17
Dependent Claim 26 words
The process of claim 1 wherein hydrolysis step (a) is carried out at ambient pressure with a solution of sodium chlorite, potassium chlorite or mixture thereof.
Claim 18
Dependent Claim 20 words
The process of claim 16 wherein the solution of sodium chlorite, potassium chlorite or mixture thereof is an aqueous solution.
Claim 19
Dependent Claim 26 words
The process of claim 16 wherein an alkali metal chlorite concentration of up to 10% by weight based on solvent and alkali metal chlorite is employed.
Claim 20
Dependent Claim 27 words
The process of claim 18 wherein an alkali metal chlorite concentration of from 2 to 6% by weight based on solvent and alkali metal chlorite is employed.
Claim 21
Dependent Claim 26 words
The process of claim 16 wherein the pH value of the solution of sodium chlorite, potassium chlorite or mixture thereof is initially adjusted to be alkaline.
Claim 22
Dependent Claim 16 words
The process of claim 20 wherein the pH value is initially adjusted to at least 11.
Claim 23
Dependent Claim 19 words
The process of claim 16 wherein hydrolysis step (a) is carried out at a temperature of 15° to 60°C.
Claim 24
Dependent Claim 19 words
The process of claim 22 wherein hydrolysis step (a) is carried out at a temperature of 30° to 55°C.
Claim 25
Dependent Claim 14 words
The process of claim 2 wherein the lignin containing residue is extracted with methanol.
Claim 26
Dependent Claim 43 words
The process of claim 2 wherein the step of treating the residue from which the lignin has been removed is carried out with alkali metal chlorite at a basic pH or with alkali metal hydroxide in the presence or absence of hydrogen peroxide.
Claim 27
Dependent Claim 12 words
The process of claim 25 wherein aqueous alkali metal hydroxide is employed.
Claim 28
Dependent Claim 13 words
The process of claim 25 wherein the alkali metal hydroxide is sodium hydroxide.
Claim 29
Dependent Claim 16 words
The process of claim 26 wherein 1 to 4% aqueous alkali metal hydroxide solution is employed.
Claim 30
Dependent Claim 11 words
The process of claim 26 carried out at 88° to 95°C.
Claim 31
Dependent Claim 28 words
The process of claim 25 wherein the residue from which the lignin has been removed is treated with alkali metal chlorite at a pH of at least 11.
Claim 32
Dependent Claim 43 words
The process of claim 2 wherein the residue from which the lignin has been extracted is treated in the presence of hydrogen peroxide with at least one member of the group consisting of alkali metal chlorite and alkali metal chloride at elevated temperature.

References Cited (Backward Citations)

US2615883A Cited
US2801955A Cited
US2835611A Cited
US3212933A Cited
US3251716A Cited
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US3817826A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-07-20 1980-01-19 1980-07-20 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-07-20 1984-01-19 1984-07-20 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-07-20 1988-01-19 1988-07-20 $7700.00 Window Closed / Lapsed

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