WO2019199823A1 - Dégommage et désuintage de matière libérienne pour la production de textile et de fibre de qualité pâte - Google Patents
Dégommage et désuintage de matière libérienne pour la production de textile et de fibre de qualité pâte Download PDFInfo
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- WO2019199823A1 WO2019199823A1 PCT/US2019/026577 US2019026577W WO2019199823A1 WO 2019199823 A1 WO2019199823 A1 WO 2019199823A1 US 2019026577 W US2019026577 W US 2019026577W WO 2019199823 A1 WO2019199823 A1 WO 2019199823A1
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- Prior art keywords
- source
- bast
- fiber
- solution
- bast fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 147
- 239000004753 textile Substances 0.000 title claims description 10
- 239000000463 material Substances 0.000 title description 11
- 238000004519 manufacturing process Methods 0.000 title description 9
- 238000009991 scouring Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000002791 soaking Methods 0.000 claims abstract description 29
- 244000025254 Cannabis sativa Species 0.000 claims abstract description 23
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims abstract description 23
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims abstract description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 23
- 235000009120 camo Nutrition 0.000 claims abstract description 23
- 235000005607 chanvre indien Nutrition 0.000 claims abstract description 23
- 239000011487 hemp Substances 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000013535 sea water Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 229920005610 lignin Polymers 0.000 claims description 29
- 244000198134 Agave sisalana Species 0.000 claims description 25
- 235000011624 Agave sisalana Nutrition 0.000 claims description 23
- 230000001590 oxidative effect Effects 0.000 claims description 16
- 229920002488 Hemicellulose Polymers 0.000 claims description 15
- 239000001814 pectin Substances 0.000 claims description 15
- 229920001277 pectin Polymers 0.000 claims description 15
- 235000010987 pectin Nutrition 0.000 claims description 15
- 229930002875 chlorophyll Natural products 0.000 claims description 13
- 235000019804 chlorophyll Nutrition 0.000 claims description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 239000011593 sulfur Substances 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 229920003043 Cellulose fiber Polymers 0.000 claims description 8
- 238000000862 absorption spectrum Methods 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 5
- 239000003599 detergent Substances 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000009954 braiding Methods 0.000 claims description 4
- 238000009950 felting Methods 0.000 claims description 4
- 239000000543 intermediate Substances 0.000 claims description 4
- 239000004745 nonwoven fabric Substances 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 239000011780 sodium chloride Substances 0.000 abstract description 9
- 241000196324 Embryophyta Species 0.000 description 12
- 229920002678 cellulose Polymers 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 10
- 235000002639 sodium chloride Nutrition 0.000 description 10
- 230000008569 process Effects 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- 239000002738 chelating agent Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- 241000208202 Linaceae Species 0.000 description 2
- 235000004431 Linum usitatissimum Nutrition 0.000 description 2
- 238000011256 aggressive treatment Methods 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000001752 chlorophylls and chlorophyllins Substances 0.000 description 2
- 239000003653 coastal water Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 235000011777 Corchorus aestuans Nutrition 0.000 description 1
- 240000004792 Corchorus capsularis Species 0.000 description 1
- 235000010862 Corchorus capsularis Nutrition 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 239000012028 Fenton's reagent Substances 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 108010059820 Polygalacturonase Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 108010093305 exopolygalacturonase Proteins 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- MGZTXXNFBIUONY-UHFFFAOYSA-N hydrogen peroxide;iron(2+);sulfuric acid Chemical compound [Fe+2].OO.OS(O)(=O)=O MGZTXXNFBIUONY-UHFFFAOYSA-N 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 235000019357 lignosulphonate Nutrition 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- -1 sulfur anion Chemical class 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C1/00—Treatment of vegetable material
- D01C1/02—Treatment of vegetable material by chemical methods to obtain bast fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
- D06L1/14—De-sizing
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/006—Pulping cellulose-containing materials with compounds not otherwise provided for
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
- D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
- D21C3/06—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides sulfur dioxide; sulfurous acid; bisulfites sulfites
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/22—Other features of pulping processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/16—Bleaching ; Apparatus therefor with per compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
- D21H11/20—Chemically or biochemically modified fibres
Definitions
- Cellulosic bast fibers harvested from plants like hemp, flax and sisal are composed of large proportions of undesired material other than cellulose, including lignin, pectin and hemicellulose, known collectively as gum. Gum serves as a natural glue adhering cellulose fibers together to provide the plant with structural rigidity. For cellulose and fiber manufacturing purposes, gum is undesired. Its presence is detrimental to the manufacturing apparatus and product quality, and undermines the efficient conversion of raw bast into marketable cellulose fiber.
- Processing bast-derived cellulose fiber requires the removal of gum through chemical and mechanical means, also known as degumming. Chemical treatments seek to target non-cellulosic molecules with minimal damage to cellulose polymers composing the fibers themselves.
- bast fiber degumming utilizes natural processes and ambient conditions to render the raw cellulose fiber and separate it from the rest of the plant - referred to as retting.
- Retting takes various forms but generally utilizes natural microbiological and chemical activity for degumming.
- cut stalks are left exposed in the field for some time.
- stalks are placed in ponds or streams.
- the fibers obtained by conventional field and water retting yield a silver-grey colored fiber due to the byproducts and staining of biological processing. Enzymatic methods and other chemical methods result in a slightly yellow or blonde to white fiber.
- Industrial scale quality-controlled degumming involves the formulation of chemical reagents and catalysts to specifically target gum and can generate problematic waste products, as well as fibers that are difficult to process.
- the present invention fulfills one or more of these needs in the art by providing a method for degumming (removal of structural non-cellulosic material) bast fibers comprising the soaking a source of bast fiber in a saline or ionic solution.
- the source of bast fibers maybe hemp.
- the source of bast fiber is soaked in a saline solution having a concentration ranging between about 1 part per thousand up to about 200 parts per thousand.
- the ion concentration of the saline solution maybe varied while the source of bast fiber is soaking in the saline solution. This step may be conducted without electrolysis of the solution.
- the source of bast fiber is soaked in seawater.
- the source of water is soaked in brackish water.
- the saline concentration may be varied over time; for example, either natural (tides) or man-made (alternating salt baths) may be used to fluctuate ion concentration. Because the ionic or saline concentration varies in water in estuaries as the tide ebbs and flows, immersing the source of bast fiber in an estuary for a series of tidal cycles can provide the salinity variations.
- the saline solution may be amended with a gum-targeting reagent.
- the method may include soaking the bast fiber in a solution containing a base to degrade lignin into water-soluble forms for removal by water.
- a basic saline solution of a base at a pH from about 7 to about 14 maybe used.
- the method may include soaking the source of bast fiber in a solution including sulfur (S oxidation number ⁇ VI) to sulfonate lignin for removal from the source of bast fiber by water.
- the source of bast fiber may be soaked in an oxidizing solution to scour lignin, pectin and hemicellulose from the source of bast fiber for removal by water.
- the method may include rinsing the source of bast fiber with detergent and surfactants to further remove lignin, pectin and hemicellulose from the source of bast fiber.
- the source of bast fiber may be mechanically agitated. For example, the source of bast fiber may tumbled.
- the present invention may also be considered a method for degumming hemp fibers from a hemp plant comprising soaking a hemp plant in a saline solution, soaking the hemp plant in a sulfur solution to sulfonate lignin for removal from hemp fiber in the hemp plant, and rinsing the hemp fiber with detergent to further remove lignin, pectin and hemicellulose from the hemp fiber.
- the method may include soaking the hemp fiber in an oxidizing solution to remove lignin, pectin and hemicellulose and their partially oxidized intermediates from the hemp fiber.
- the hemp fiber may be soaked in a hydrogen peroxide solution.
- the hydrogen peroxide and other oxidant sources maybe generated in situ e.g. via electrolysis.
- the hemp fiber may be soaked in the oxidizing solution at a pH between about 6 to about 14 and at a temperature below a boiling point of the oxidizing solution. This step may be conducted without electrolysis of the solution.
- the hemp fiber may be soaked in the sulfur solution at a pH between about 6 to about 14 and at a temperature between ambient (20-30°C) to about 95°C.
- soaking the hemp plant in a saline solution comprises soaking the hemp plant directly into or within a vessel connected to natural, tidally flushed coastal waters so that the ionic composition and associated alkalinity, acidity, and density of the solution proximate to the hemp plant varies with tidal fluctuations.
- the resulting fiber is suitable for spinning into textile-quality yam using conventional textile methods and machinery, wherein the processing is selected from the group consisting of making a yam by spinning, braiding, felting, making nonwovens such as by needle-punching, and more than one of them. Bleaching or oxidation need not be used, eliminating the inherent production of potentially toxic by-products by this method and allows the bast material to retain elements of its original natural green color.
- the fiber (fiber containing chlorophyll), thus degummed, maintains at least some of its green color and is sufficiently free of lignin, pectin, and hemicellulose, and the fiber can be processed in conventional textile machinery, wherein the processing is selected from the group consisting of making a yam by spinning, braiding, felting, making nonwovens such as by needle-punching, and more than one of them.
- the green color of the bast fiber is typically imparted to the bast fiber by chlorophyll.
- the bast fiber may be hemp.
- the source of green color of the bast fiber may, upon extraction into a solvent, show a photometric absorption spectrum indicative of general chlorophyll pigments (Chi a, b & c).
- a photometric absorption spectrum indicative of general chlorophyll pigments (Chi a, b & c).
- Chi a, b & c general chlorophyll pigments
- Jeffrey and Humphrey “New Spectrophotometric Equations for Determining Chlorophylls a, b, ci, c 2 in Higher Plants, Algae and Natural Phytoplankton,” Biochem. Physiol. De (BPP) Bd 167, S. 191-194 (1975)
- data from 750, 664, 647 and 630 nm wavelengths can be used to calculate chlorophyll concentration directly from a suitable absorption spectrum.
- a 500 mg sample of green-colored, degummed, hemp fiber sample produced in accordance with an embodiment of the method was soaked in 100 mL of deionized water for 12 hours and filtered through a 0.45 mhi Supor membrane.
- Data from an absorption spectrum per Jeffrey and Humphrey (1975) showed 1.6 mg/L total chlorophyll in the extract, equivalent to at least 0.03% chl in the fiber sample by mass.
- Figure 1 is a black and white photograph of four samples.
- the present invention is directed to a method for processing plants that include bast fibers to remove lignin, pectin and hemicellulose (collectively referred to as“gum”) and other undesirable materials.
- the result is a cellulose fiber partially, mostly, or wholly free from gum so that it may be used in manufacturing for conversion into marketable materials such as textile fibers.
- the bast fibers may be hemp, flax or sisal. Jute and other fibers are also known as bast fibers.
- the method comprises soaking a plant that is a source of bast fibers in a saline solution.
- the source of bast fiber may be soaked and agitated in a brine solution.
- the source of bast fiber may be soaked and agitated in an alkaline solution.
- the source of bast fiber may be soaked and agitated in solution with a pH > 6, and this is typically performed without electrolysis of the solution.
- the solution is comprised of water and inorganic salt with a total salinity ranging from less than 1 to about 200 parts per thousand (ppt).
- Salinity sources can include those found naturally such as in tidally flushed estuaries, creeks, coastal and sea water.
- Natural freshwater can be used, though consideration for ionic discharge into freshwater watersheds should be made.
- freshwater has a salinity ranging from about 0 to about 0.5 ppt
- brackish waters has a salinity ranging from about 0.5 ppt to about 30 ppt
- seawater has a salinity ranging from about 30 ppt to about 50 ppt.
- the submersion of the source of bast fibers into an aqueous solution leads to uptake of water and aqueous ions into interstices between cellulosic fibers and gum and into the cellulose matrix due to cellulose wetting and capillary action. This imparts a pressure on the cellulose structure causing it to swell.
- the presence of ions in solution within the cellulose matrix alters the wetting behavior of cellulose, alters the capillary and pore pressures, and enhances interstitial transport and swelling. Swelling imparts mechanical stress on the bast structure, helps expose the fiber body to reagent, increases substrate surface area, delivers reagent for subsequent steps, and enhances fiber separation.
- ion concentration reduces the swelling behavior, enhances diffusive export of dissolved material from the cellulose matrix (effectively flushing it), and imparts stress on the fiber matrix, further enhancing separation.
- the process may be enhanced through additional mechanical treatment.
- Interstitial pressure gradients may be sustained by periodic increase and decrease in the ion concentration of the solution, through salt or brine addition or dilution, and will enhance fiber separation as well as exposure of gum to reagent.
- the use of tidally-flushed estuarine water sources permits the naturally available and non-interfering use of sea salt as a source of interstitial pressure.
- the use of tidally flushed water in an estuary also removes gum and/or its partially oxidized intermediates from the bast fibers safely through flushing.
- Exposing the source of bast fiber to the variations in ion concentration can be carried out under increased temperature and pressure to enhance diffusion and reaction rates, and increase interstitial pressures.
- the method may also include exposing lignin present in the bast fiber to a degumming reagent.
- a degumming reagent may include a base to depolymerize lignin into smaller, lighter weight, soluble lignin products.
- a basic saline solution of a base at a pH from about 7 to about 14 may be used.
- the method may also include sulfonating the lignin present on the bast fiber to create water-soluble products that can be removed by flushing the bast fiber with water.
- a neutral to alkaline solution of strong base and a sulfur anion at a pH from about 7 to about 14 may be used. Sulfur in neutral to alkaline solution will react with ring structures in lignin to yield a sulfonated soluble product readily removed from the plant material through flushing.
- Sufficient sulfur is provided to account for the range of lignin content of the source of bast fiber (generally 5-15% lignin by mass for raw fiber, and less for retted or otherwise pre-processed fiber).
- the source of bast fiber maybe soaked in a sulfonating solution for 10 minutes to several hours at pressure ranging from ambient to 10 atmospheres. Temperatures may vary with pressure per the Clausius- Clapyeron relation.
- the bast fibers may also be soaked in an oxidizing solution to bleach the fibers and scour remaining gum.
- the oxidant may be added to the solution directly or generated in situ (e.g. by electrolysis).
- the addition of oxidant stabilizers may be included in some embodiments.
- the needed water temperature and soak time are dependent on the oxidant used.
- a water solution with a pH ranging from about 8 to about 12 is made with a combination of a strong base and a buffer.
- 50 mL of 3% 3 ⁇ 4(3 ⁇ 4 is added to a solution of 2 g/L NaOH and 1 g/L NaHC0 3 .
- the hemp fiber is soaked from about 0.1 to about 1 hour at a temperature below the boiling point of the solution. Since some naturally occurring heavy metals (Fe, Mg) interfere with 3 ⁇ 4(3 ⁇ 4 oxidation of gum (e.g. see Fenton’s Reagent), the addition of chelators may be used to prohibit or minimize their interference. Additional steps may also be added to further degum the hast fibers. For example detergent may be used to rinse and remove any remaining soluble, partially soluble, or insoluble (but mobile) gum in the bast fiber. Pectinase or other natural enzymes (either directly added or through in situ biological production) may be used as a non-essential component to assist in the removal of gum from the bast fibers. The steps may include mechanical agitation. Mechanical agitation may be tumbling, stirring or other agitation.
- the steps for degumming the bast fibers may vary depending upon the chemical and physical conditions of the water source.
- Potential sources of water for soaking the bast fibers include most natural waters as well as municipal and purified water. Since the method utilizes saline solutions, sources of naturally saline water may be used to advantage.
- Raw water may be used in one or more steps.
- Some natural sources of water contain components that may be utilized as reagents for one or more of the steps described above.
- waters available from wetlands contain naturally abundant sulfur (i.e., having an oxidation number less than or equal to VI) that can be used for sulfonating lignin.
- the presence of naturally available reactants or reagent components within the water source may be accounted for when formulating the desired reagent composition.
- naturally available chelators may be used in place of manually added ones.
- the natural salinity of the water source may be accounted for in all steps, and its natural salinity variability (due to tides or other factors) may be used as a source of enthalpy for physical and chemical processing.
- Naturally available alkaline water sources may also be useful for certain processes wherein the pH of the solution is within a range from about 8 to about 12.
- the bast fibers may be pretreated or decorticated, thus requiring a less aggressive treatment. Certain steps may be repeated (with or without a more aggressive reagent) if it is determined by an operator that the results of one or more steps are deemed insufficient. In some examples, the plant stalks may still be intact (i.e. the bast is not separated from the whole plant), requiring additional steps/repetitions to remove additional gum. On the other hand, some sources of bast fibers may be already be partially processed (“retted”) and require a less aggressive treatment, permitting omission of one or more steps. Material of a specified quality due to variable control available to the method may also be desired.
- the effluent from the degumming process may be a solution and mixture of gum, its partially oxidized intermediates, and its oxidation byproducts, residual cellulose fiber lost due to agitation, as well as inorganic salts, residual reagent, detergent, and chelators.
- Post-treatment of effluent includes additional oxidation (through addition of oxidants and/or in situ generation) or biological activity, per standard municipal water treatment protocols. Residual fiber, lignin and sulfonated lignin may be recovered from the effluent as marketable material. Suitable, detoxified effluent may be used as a nutrient additive to soils for agriculture.
- Inorganic ions may be added to the effluent to adjust ion ratios and salinity to match that of surface waters into which effluent will be discharged.
- Effluent alkalinity or acidity may be neutralized through titration with a suitable acid or base.
- the fiber obtained by the process outlined above is a high-quality, separated, soft, spinnable fiber.
- the bast fiber is sufficiently free of lignin, pectin and hemicellulose that the fiber can be processed in conventional textile machinery. Such processing can include making a yam by spinning, braiding, felting, and making nonwovens such as by needle-punching.
- the bast fiber may retain a green color.
- the color can be ascertained by extraction of the bast fiber into a solvent, showing a photometric absorption spectrum indicative of general chlorophyll pigments (Chl a, b & c). As described in Jeffrey and Humphrey,“New
- Figure 1 is a black and white photograph of four samples. From left to right these samples are:
- the method disclosed herein is not limited to the order described above.
- the above steps may be omitted, repeated, combined, or carried out in a different order.
- limited resources may require combining steps, or reusing effluent from one step in another.
- the step order, parameters and iterations maybe modified in some embodiments to enhance or diminish specific fiber properties or composition, or to unify the properties of the end product relative to those of the unprocessed bast. It should be understood that all such modifications and improvements have been omitted for the sake of conciseness and readability, but are properly within the scope of the following claims.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Zoology (AREA)
- Inorganic Chemistry (AREA)
- Biochemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Paper (AREA)
Abstract
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19786218.8A EP3765659A4 (fr) | 2018-04-09 | 2019-04-09 | Dégommage et désuintage de matière libérienne pour la production de textile et de fibre de qualité pâte |
MX2020010328A MX2020010328A (es) | 2018-04-09 | 2019-04-09 | Desgomado y descrudacion de material liberiano para la produccion de fibra textil y de calidad de pulpa. |
US17/044,605 US20210148009A1 (en) | 2018-04-09 | 2019-04-09 | Degumming and scouring of bast material for production of textile and pulp-quality fiber |
CA3096348A CA3096348A1 (fr) | 2018-04-09 | 2019-04-09 | Degommage et desuintage de matiere liberienne pour la production de textile et de fibre de qualite pate |
AU2019251227A AU2019251227A1 (en) | 2018-04-09 | 2019-04-09 | Degumming and scouring of bast material for production of textile and pulp-quality fiber |
CN201980037888.7A CN112616316A (zh) | 2018-04-09 | 2019-04-09 | 用于纺织和浆质量纤维的生产的韧皮材料的脱胶和洗刷 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US201862654573P | 2018-04-09 | 2018-04-09 | |
US62/654,573 | 2018-04-09 |
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WO2019199823A1 true WO2019199823A1 (fr) | 2019-10-17 |
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Application Number | Title | Priority Date | Filing Date |
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PCT/US2019/026577 WO2019199823A1 (fr) | 2018-04-09 | 2019-04-09 | Dégommage et désuintage de matière libérienne pour la production de textile et de fibre de qualité pâte |
Country Status (7)
Country | Link |
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US (1) | US20210148009A1 (fr) |
EP (1) | EP3765659A4 (fr) |
CN (1) | CN112616316A (fr) |
AU (1) | AU2019251227A1 (fr) |
CA (1) | CA3096348A1 (fr) |
MX (1) | MX2020010328A (fr) |
WO (1) | WO2019199823A1 (fr) |
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CN115386969B (zh) * | 2022-09-16 | 2024-01-30 | 江南大学 | 一种des溶剂协同碱氧对大麻纤维进行脱胶的方法 |
Citations (5)
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US2026584A (en) | 1935-01-11 | 1936-01-07 | Joseph A Manahan | Method of liberating fibers |
US20080020449A1 (en) * | 2004-01-06 | 2008-01-24 | Hironori Matsubara | Method For Separating Bast Fibers |
US20090092835A1 (en) * | 2005-11-01 | 2009-04-09 | Xu Meirong | Bast fibers obtained from an extraction and preparation process |
US20100147472A1 (en) * | 2006-06-08 | 2010-06-17 | Sung Wing L | Extraction of hemp fibers |
CN101768785B (zh) * | 2008-12-30 | 2013-02-27 | 季英超 | 渐进式麻纤维脱胶方法 |
Family Cites Families (8)
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CN85105350B (zh) * | 1985-06-28 | 1987-10-28 | 山东省东平县麻纺厂 | 大麻化学脱胶工艺 |
CN100500954C (zh) * | 2007-07-10 | 2009-06-17 | 浙江理工大学 | 一种大麻海水沤麻与低碱联合脱胶方法 |
CN101148782B (zh) * | 2007-09-10 | 2010-08-11 | 中国人民解放军总后勤部军需装备研究所 | 一种麻类韧皮纤维闪爆—高温蒸煮联合脱胶工艺方法 |
KR100861457B1 (ko) * | 2008-07-30 | 2008-10-02 | 정일훈 | 미생물을 이용한 인피섬유 및 그 제조방법 |
CN102330158B (zh) * | 2011-08-09 | 2013-04-24 | 太原理工大学 | 一种汉麻脱胶与柔顺同步处理工艺 |
CN105256383A (zh) * | 2015-11-12 | 2016-01-20 | 六安市华龙麻纺工艺制品有限公司 | 一种黄麻脱胶方法 |
CN106567138B (zh) * | 2016-10-27 | 2018-09-18 | 青岛大学 | 一种大麻纤维的精细化加工方法 |
CN106868862B (zh) * | 2017-03-21 | 2019-02-22 | 张辰龙 | 一种可纺度高的抗静电大麻纤维的制备方法 |
-
2019
- 2019-04-09 US US17/044,605 patent/US20210148009A1/en not_active Abandoned
- 2019-04-09 CA CA3096348A patent/CA3096348A1/fr active Pending
- 2019-04-09 AU AU2019251227A patent/AU2019251227A1/en not_active Withdrawn
- 2019-04-09 CN CN201980037888.7A patent/CN112616316A/zh active Pending
- 2019-04-09 EP EP19786218.8A patent/EP3765659A4/fr active Pending
- 2019-04-09 WO PCT/US2019/026577 patent/WO2019199823A1/fr active Application Filing
- 2019-04-09 MX MX2020010328A patent/MX2020010328A/es unknown
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US2026584A (en) | 1935-01-11 | 1936-01-07 | Joseph A Manahan | Method of liberating fibers |
US20080020449A1 (en) * | 2004-01-06 | 2008-01-24 | Hironori Matsubara | Method For Separating Bast Fibers |
US20090092835A1 (en) * | 2005-11-01 | 2009-04-09 | Xu Meirong | Bast fibers obtained from an extraction and preparation process |
US20100147472A1 (en) * | 2006-06-08 | 2010-06-17 | Sung Wing L | Extraction of hemp fibers |
CN101768785B (zh) * | 2008-12-30 | 2013-02-27 | 季英超 | 渐进式麻纤维脱胶方法 |
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See also references of EP3765659A4 |
Also Published As
Publication number | Publication date |
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CA3096348A1 (fr) | 2019-10-17 |
EP3765659A4 (fr) | 2022-06-01 |
MX2020010328A (es) | 2020-12-10 |
EP3765659A1 (fr) | 2021-01-20 |
AU2019251227A1 (en) | 2020-10-29 |
US20210148009A1 (en) | 2021-05-20 |
CN112616316A (zh) | 2021-04-06 |
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