# US 11,439,160 B2 · Method for producing hydrolysed keratinaceous material

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- Number: US 11,439,160 B2
- Document ID: US11439160B2
- Status: Granted
- Kind: B2
- Application number: 14/908,564
- Filed: 2014-07-29
- Published: 2016-06-09
- Granted: 2022-09-13
- Earliest claimed: 2013-07-30
- Assignees: Tessenderlo Chemie S.A.
- Applicants: Tessenderlo Chemie N.V.
- Inventors: Romain Fillières; Marc Belmans; Frank Boers; Faye Maertens; Joeri Rogiers
- Web page: https://patentgrep.com/patent/US11439160B2

## CPC

- A23J 3/32: using chemical agents
- A23J 1/10: from hair, feathers, horn, skins, leather, bones, or the like
- A23J 3/30: by hydrolysis
- A23L 33/18: Peptides; Protein hydrolysates
- A61K 8/65: Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
- A61Q 19/00: Preparations for care of the skin
- C08H 1/06: derived from horn, hoofs, hair, skin or leather
- A23V 2002/00: Food compositions, function of food ingredients or processes for food or foodstuffs
- A61K 2800/10: General cosmetic use
- A23J: PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- C08H: DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS (polysaccharides C08B; natural rubber C08C; natural resins or their derivatives C09F; bituminous materials C10)
- A23V: INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION

## Abstract

The method of the invention comprises the production of highly digestible hydrolysed keratinaceous material comprising the steps of (i) partly hydrolysing keratinaceous material with heat and pressure and (ii) optionally drying the resultant partly hydrolysed material comprising at least partly insoluble material and (iii) subjecting the optionally dried partly hydrolysed keratinaceous material to a chemical hydrolysis step with acid or base to obtain a highly digestible hydrolysed material, and (iv) purifying the highly digestible material. The invention further provides highly digestible keratinaceous material with an amino acid composition reflecting the amino acid composition of the raw material, wherein the amount of de-carboxylated amino acids is less than 500 ppm. Preferably all of the highly digestible material has a molecular weight lower than 10000 dalton, and preferably more than 95 wt % of the highly digestible keratinaceous material has a molecular weight of less than 5000 dalton.

## Claims

### Claim 1

A method for the production of a digestible hydrolysed material, comprising the steps of
(i) partly hydrolysing a keratinaceous material in the presence of water with heat and pressure wherein the hydrolysis reaction is performed with only water/steam as the active reagent at a pressure of 4 bar absolute or higher, to obtain partly hydrolysed keratinaceous material which comprises—when dissolved in water/acetonitrile/TFA—about 40 wt % or more of material that has a molecular weight of about 5000 dalton or less, and about 20 wt % or more of material having a molecular weight of about 5000 dalton or higher, and
(ii) subjecting the partly hydrolysed keratinaceous material to a chemical hydrolysis step with an strong mineral acid to obtain the digestible hydrolysed material, and
(iii) purifying the digestible hydrolysed material,
wherein the digestible hydrolysed material has 90% by weight or more of material of a molecular weight of 1000 dalton or lower, and an in vitro ileal digestibility of 98% or more, and an in vitro pepsin digestibility of 98% or more.

### Claim 2 (depends on 1)

The method according to claim 1, wherein in step (i) the keratinaceous material is hydrolysed at a pressure between 4 bar absolute and about 15 bar absolute, during about 5 to about 240 min.

### Claim 3

A method for the production of a digestible hydrolysed material comprising the steps of subjecting a partly hydrolysed, partly insoluble keratinaceous material to a further chemical hydrolysis step,
wherein the partly hydrolysed, partly insoluble keratinaceous material comprises—when dissolved in water/acetonitrile/TFA—about 40 wt % or more of material that has a molecular weight of about 5000 dalton or less, and about 20 wt % or more of material having a molecular weight of about 5000 dalton or higher, obtained from thermal and pressure hydrolysis,
wherein the hydrolysis reaction is performed with only water/steam as the active reagent at a pressure of 4 bar absolute or higher, and
wherein the further chemical hydrolysis step comprises chemical hydrolysis with an strong mineral acid to obtain the digestible hydrolysed material, and purifying the digestible hydrolysed material wherein the digestible material has 90% by weight or more of material of a molecular weight of 1000 dalton or lower and an in vitro ileal digestibility of 98% or more, and an in vitro pepsin digestibility of 98% or more.

### Claim 4

A method for the production of a digestible hydrolysed keratinaceous material comprising subjecting a partly hydrolysed keratinaceous material with a moisture content of about 10 wt % or less to a chemical hydrolysis step,
wherein the partly hydrolysed keratinaceous material is a keratinaceous meal,
wherein the partly hydrolysed keratinaceous material comprises—when dissolved in water/acetonitrile/TFA—about 40 wt % or more of material that has a molecular weight of about 5000 dalton or less, and about 20 wt % or more of material having a molecular weight of about 5000 dalton or higher,
wherein the chemical hydrolysis step comprises chemical hydrolysis with a strong mineral acid to achieve the digestible hydrolysed keratinaceous material, and purifying the digestible hydrolysed keratinaceous material wherein the digestible material has 90% by weight or more of material of a molecular weight of 1000 dalton or lower and an in vitro ileal digestibility of 98% or more, and an in vitro pepsin digestibility of 98% or more.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the strong mineral acid is sulphuric acid.

### Claim 6 (depends on 5)

The method according to claim 5, wherein the purification (iii) of the digestible hydrolysed material is performed while forming a salt by neutralisation and separating the salt from the digestible hydrolysed material, wherein the salt is calcium sulphate dihydrate, which is removed.

### Claim 7 (depends on 1)

The method according to claim 1, wherein a solution comprising the digestible hydrolysed material is converted to a concentrated solution comprising about 30-60 wt % solids.

### Claim 8 (depends on 1)

The method according to claim 1, wherein a solution comprising the digestible hydrolysed material is converted to a solid.

### Claim 9 (depends on 1)

A digestible hydrolysed keratinaceous material, obtainable with the method of claim 1, wherein the digestible hydrolysed keratinaceous material has an amino acid composition reflecting the amino acid composition of the keratinaceous material, wherein an amount of de-carboxylated amino acids is less than about 1000 ppm, and wherein the digestible keratinaceous material has 90% by weight or more of material of a molecular weight of 1000 dalton or lower and an in vitro ileal digestibility of 98% or more, and an in vitro pepsin digestibility of 98% or more.

### Claim 10 (depends on 9)

The digestible hydrolysed keratinaceous material according to claim 9, wherein the digestible hydrolysed keratinaceous material contains lanthionine in an amount of about 2.0 wt % or less.

### Claim 11 (depends on 9)

The digestible hydrolysed keratinaceous material according to claim 9, wherein the digestible hydrolysed keratinaceous material has an in vivo digestibility of the Total Nitrogen Matter of about 82% or more, as determined on cecectomized roosters.

### Claim 12 (depends on 1)

The method according to claim 1, wherein step (i) further comprises drying the partly hydrolysed keratinaceous material and wherein step (ii) comprises subjecting the dried partly keratinaceous hydrolysed material to the chemical hydrolysis step with a strong mineral acid to obtain the digestible hydrolysed material.

### Claim 13 (depends on 1)

A feed or feed additive comprising the digestible hydrolysed material obtained according to claim 1, wherein the digestible hydrolysed material has an amino acid composition reflecting the amino acid composition of the keratinaceous material wherein the deviation in amino acid composition of the digestible hydrolysed material and the keratinaceous material is less than 20% in the amino acids, and/or a deviation in an amount absolute of less than 0.4 wt % in the amino acids, whereby up to 3 amino acids deviate to a maximum of 40% or 2 wt %, and wherein an amount of de-carboxylated amino acids is less than about 1000 ppm.

### Claim 14 (depends on 12)

The method according to claim 12, wherein the drying in step (i) is performed at a temperature below 80° C.