Processes to Prepare Highly Functional Fiber Products and Products Produced Thereby
Processes to prepare highly functional fiber products from agricultural by-products (e.g., sugar beet pulp, orange peel, apple pulp and other pectin containing agricultural processing by-products) and their applications are disclosed. Sequential extraction of pectin from agricultural by-products produced a series of fractions with excellent oil in water emulsification and water holding capacity properties.
1 . A process for making pectin F1, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) combining said washings and said acid extracted filtrate to form combined filtrate and washings and adjusting the pH of said combined filtrate and washings to about 3 to about 3.2, and
(9) adding alcohol to said combined filtrate and washings to precipitate said pectin F1, and
(10) isolating said pectin F1.
2 . A process for making pectin F2, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) rinsing said washed residue with an alcohol to form a rinsed residue,
(9) mixing said rinsed residue with water and adjusting the pH to about 6.8 and adding α-amylase to form a slurry,
(10) adjusting the pH of said slurry to about 11.5 and stirring,
(11) shearing said slurry,
(12) separating said slurry into an alkali insoluble solid residue and an alkali solubilized fraction which contains pectin F2 and pectin F3, and
(13) adjusting the pH of said alkali solubilized fraction to about 4 to form pectin F2, and
(14) isolating pectin F2.
3 . A process for making pectin F3, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) rinsing said washed residue with an alcohol to form a rinsed residue,
(9) mixing said rinsed residue with water and adjusting the pH to about 6.8 and adding α-amylase to form a slurry,
(10) adjusting the pH of said slurry to about 11.5 and stirring,
(11) shearing said slurry,
(12) separating said slurry into an alkali insoluble solid residue and an alkali solubilized fraction which contains pectin F2 and pectin F3, and
(13) adjusting the pH of said alkali solubilized fraction to about 4 which precipitates pectin F2, and
(14) isolating pectin F3 from pectin F2.
4 . A process for making acid and alkali soluble materials, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) rinsing said washed residue with an alcohol to form a rinsed residue,
(9) mixing said rinsed residue with water and adjusting the pH to about 6.8 and adding α-amylase to form a slurry,
(10) adjusting the pH of said slurry to about 11.5 and stirring,
(11) shearing said slurry,
(12) separating said slurry into an alkali insoluble solid residue and an alkali solubilized fraction which contains pectin F2 and pectin F3,
(13) adjusting the pH of said alkali solubilized fraction to about 4, (14) centrifuging or filtering said alkali solubilized fraction to separate and isolate pectin F2 from the supernatant or filtrate containing pectin F3,
(15) adding alcohol to said supernatant or filtrate to form a first precipitate and first decantant,
(16) removing said first precipitate and adding alcohol to form a second precipitate and second decantant, and
(17) combining said first decantant and said second decantant which contains said acid and alkali soluble materials.
5 . A process for making cellulosic fraction F4, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) rinsing said washed residue with an alcohol to form a rinsed residue,
(9) mixing said rinsed residue with water and adjusting the pH to about 6.8 and adding α-amylase to form a slurry,
(10) adjusting the pH of said slurry to about 11.5 and stirring,
(11) shearing said slurry,
(12) separating said slurry into an alkali insoluble solid residue and an alkali solubilized fraction which contains pectin F2 and pectin F3,
(13) suspending said alkali insoluble solid residue in boiling water and stirring,
(14) shearing said alkali insoluble solid residue to form a first sheared material,
(15) cooling said first sheared material to about room temperature and centrifuging to separate solid residue 1,
(16) suspending said solid residue 1 in boiling water and stirring,
(17) shearing said solid residue 1 to form a second sheared material,
(18) centrifuging said second sheared material to separate solid residue 2,
(19) suspending said solid residue 2 in boiling water and stirring,
(20) shearing said solid residue 2 to form a third sheared material,
(21) centrifuging said third sheared material to separate solid residue 3,
(22) suspending said solid residue 3 in boiling water and stirring,
(23) shearing said solid residue 3 to form a fourth sheared material, and
(24) cooling said fourth sheared material to about room temperature and centrifuging to separate and isolate solid residue 4 which contains cellulosic fraction F4.
6 . A process for making a hot water extract, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass and a liquid filtrate from said de-oiled biomass, and
(3) removing water from said liquid filtrate to form said hot water extract.
7 . A process for making materials having a molecular weight less than 30 KDa, said process comprising:
(1) removing oil from an agricultural by-product to form a de-oiled biomass,
(2) adding hot water with stirring to said de-oiled biomass and separating a hot water extracted biomass from said de-oiled biomass,
(3) removing water from said hot water extracted biomass to form a dry product,
(4) adding water to said dry product to form a suspension and adjusting the pH of said suspension to about 1.6,
(5) heating said suspension with stirring,
(6) cooling said suspension to about room temperature and separating said suspension to produce an acid extracted residue and an acid extracted filtrate,
(7) washing said acid extracted residue with water to form washings and a washed residue,
(8) combining said washings and said acid extracted filtrate to form combined filtrate and washings and adjusting the pH of said combined filtrate and washings to about 3 to about 3.2, and
(9) adding alcohol to said combined filtrate and washings to precipitate said pectin F1,
(10) isolating said pectin F1 to form isolated pectin F1 and a final filtrate, and
(11) evaporating said final filtrate to from materials having a molecular weight less than 30 KDa.
8 . Pectin F1, said pectin F1 produced by the process of claim 1 .
9 . Pectin F2, said pectin F2 produced by the process of claim 2 .
10 . Pectin F3, said pectin F3 produced by the process of claim 3 .
11 . Acid and alkali soluble materials, said acid and alkali soluble low molecular weight materials produced by the process of claim 4 .
12 . Cellulosic fraction F4, said cellulosic fraction F4 produced by the process of claim 5 .
13 . How water extract, said hot water extract produced by the process of claim 6 .
14 . Materials having a molecular weight less than 30 KDa, said materials produced by the process of claim 7 .