Method for production of cellulose nano crystals from cellulose-containing waste material
US-9464142-B2 · Oct 11, 2016 · US
US10000579B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10000579-B2 |
| Application number | US-201415109232-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 30, 2014 |
| Priority date | Dec 30, 2013 |
| Publication date | Jun 19, 2018 |
| Grant date | Jun 19, 2018 |
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An integrated process for the recovery of a spectrum of commercially valuable products such as agar, cellulose, lipids, pigments and a liquid rich in minerals of agricultural importance directly from fresh seaweed without employing any catalyst driven in situ chemical conversions. Also solvents used during lipid extraction were shown to be used for three cycles without affecting the yield and quality of successive products. Furthermore, this new process is highly efficient and utilizes total seaweed raw material without any leftover biomass as solid waste.
Opening claim text (preview).
We claim: 1. An integrated process to recover a spectrum of bioproducts from fresh seaweeds, the process comprising the steps of: performing an aqueous extraction on the fresh seaweeds to from a first residue and a supernatant; and performing a solvent extraction on the first residue to recover a lipid product and a second residue, wherein the step of performing an aqueous extraction comprises: homogenizing the fresh seaweeds in a phosphate buffer having a pH in the range of 6.8 to 7.0; incubating the homogenized fresh seaweeds at a temperature in the range of 4 to 6 degree C. for a time period of 10 to 12 hours; separating the first residue and the supernatant with a centrifuge, the centrifuge operating from 5000 to 7000 rpm for a period of 12 to 15 minute, the separation occurring at a temperature of 4 to 10 degree C., wherein the step of performing a solvent extraction comprises: extracting the lipid product from the first residue using chloroform and methanol mixed in a ratio of 1:2 v/v; separating the lipid product from the second residue with a centrifuge operating from 4000 to 5000 rpm for a period of 10 to 15 minutes, the separation occurring at a temperature of 4 to 10° C., and wherein the supernatant comprises pigments and protein. 2. The integrated process of claim 1 , further comprising: precipitating the pigments from the supernatant with ammonium sulphate; and separating the precipitated pigments with a centrifuge, the centrifuge operating from 6500 to 8000 rpm for a period of 12 to 15 minutes, the precipitated pigment separation occurring at a temperature of 4 to 10 degrees C. 3. The integrated process of claim 1 , further comprising: filtering the supernatant with a membrane filter to concentrate the pigments. 4. The integrated process of claim 1 , wherein the fresh seaweeds comprises an agarophyte. 5. The integrated process of claim 4 , further comprising: performing a polysaccharide extraction process on the second residue to recover an agar product and a third residue. 6. The integrated process of claim 5 , wherein the step of performing a polysaccharide extraction process further comprises: drying the second residue at a temperature in the range of 60 to 65 degree C. for 50 to 60 minutes; cooking the dried second residue in a cooking solution of fresh algal biomass and distilled water present in a ratio of 1:5 w/v at a temperature of 115 to 120 degree C. for 80 to 90 minutes; homogenizing the cooked second residue with a mixer grinder; and separating an agar supernatant and the third residue with a centrifuge operating at 6000 to 7000 rpm for a period of 4 to 6 minutes, the separation occurring at a temperature of 40 to 60 degrees C. 7. The integrated process of claim 6 , further comprising: forming a gel of the agar supernatant at a temperature of 25 to 30 degrees C.; freezing the gel at a temperature of −15 to −20 degrees C. for 12 to 15 hours; thawing the frozen gel to obtain the agar product; and drying the agar product at a temperature of 60 to 65 degrees C. for 10 to 12 hours. 8. The integrated process of claim 1 , wherein the fresh seaweeds comprise a carrageenophyte. 9. The integrated process of claim 8 , further comprising: performing a polysaccharide extraction process on the second residue to recover a carageenan product and a third residue. 10. The integrated process of claim 9 , wherein the step of performing a polysaccharide extraction process further comprises: drying the second residue at a temperature in the range of 60 to 65 degree C. for 50 to 60 minutes; cooking the dried second residue in an 8% KOH solution at a temperature of 70 to 72 degrees C. for 105 to 120 minutes; filtering the cooked second residue; washing the filtered second residue with tap water; cooking the washed second residue with water at a temperature of 75 to 78 degrees C. for 40 to 45 minutes; homogenizing the cooked second residue and separating the cooked second residue into a cooked supernatant and the third reside with a centrifuge operating at 6000 to 7000 rpm for 3 to 5 minutes; precipitating carageenan from the cooked supernatant in chilled isopropanol; and drying the precipitated carrageenan at a temperature of 60 to 65 degrees C. for 4 to 6 hours. 11. The integrated process of claim 5 further comprising: performing a cellulosic extraction process on the third residue to recover a cellulose product. 12. The integrated process of claim 10 , wherein the step of performing a cellulosic extraction process further comprises: drying the third residue; soaking the third residue in an acetate buffer having a pH of 4.5 containing 36% NaClO 2 (w/w) for bleaching of the third residue; washing the bleached third residue with water; treating the washed third residue with a 0.5 M NaOH solution at a temperature of 60 to 65 degree C. for 10 to 12 hours; washing with water to form a neutralized material; drying the neutralized material; treating the dried neutralized material with a 5% (v/v) solution of hydrochloric acid to form a treated material; boiling the treated material; incubating the boiled treated material at a temperature of 25 to 30 degrees C. for 10 to 14 hours to form a slurry; washing the slurry with water; and drying the slurry to form the cellulose product. 13. The integrated process of claim 9 further comprising: performing a cellulosic extraction process on the third residue to recover a cellulose product. 14. The integrated process of claim 13 , wherein the step of performing a cellulosic extraction process further comprises: drying the third residue; soaking the third residue in an acetate buffer having a pH of 4.5 containing 36% NaClO 2 (w/w) for bleaching of the third residue; washing the bleached third residue with water; treating the washed third residue with a 0.5 M NaOH solution at a temperature of 60 to 65 degree C. for 10 to 12 hours; washing with water to form a neutralized material; drying the neutralized material; treating the dried neutralized material with a 5% (v/v) solution of hydrochloric acid to form a treated material; boiling the treated material; incubating the boiled treated material at a temperature of 25 to 30 degrees C. for 10 to 14 hours to form a slurry; washing the slurry with water; and drying the slurry to form the cellulose product.
Cross-Sectional Technologies · mapped topic
General processes for their isolation or fractionation, e.g. purification or extraction from biomass · CPC title
Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds · CPC title
Carragenan or carragen, i.e. D-galactose and 3,6-anhydro-D-galactose, both partially sulfated, e.g. from red algae Chondrus crispus or Gigantia stellata; kappa-Carragenan; iota-Carragenan; lambda-Carragenan; Derivatives thereof · CPC title
produced by the action of a carbohydrase {(EC 3.2.x)}, e.g. by alpha-amylase {, e.g. by cellulase, hemicellulase} · CPC title
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