EP3697950A1 - Method for producing wood-based yarn filaments - Google Patents
Method for producing wood-based yarn filamentsInfo
- Publication number
- EP3697950A1 EP3697950A1 EP18804034.9A EP18804034A EP3697950A1 EP 3697950 A1 EP3697950 A1 EP 3697950A1 EP 18804034 A EP18804034 A EP 18804034A EP 3697950 A1 EP3697950 A1 EP 3697950A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- des
- solvent
- cellulose
- pulp
- cellulosic material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002023 wood Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 230000005496 eutectics Effects 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 18
- 229920002678 cellulose Polymers 0.000 claims description 17
- 239000001913 cellulose Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 14
- 235000019743 Choline chloride Nutrition 0.000 claims description 14
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 14
- 229960003178 choline chloride Drugs 0.000 claims description 14
- 239000000835 fiber Substances 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- 229920001046 Nanocellulose Polymers 0.000 claims description 2
- 239000011121 hardwood Substances 0.000 claims description 2
- 239000011859 microparticle Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 125000003158 alcohol group Chemical group 0.000 claims 1
- 238000001125 extrusion Methods 0.000 abstract description 4
- 239000004753 textile Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 238000013478 data encryption standard Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WLJVXDMOQOGPHL-PPJXEINESA-N 2-phenylacetic acid Chemical compound O[14C](=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-PPJXEINESA-N 0.000 description 1
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229960005150 glycerol Drugs 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 229940116315 oxalic acid Drugs 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 229940045136 urea Drugs 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
Definitions
- the present invention relates to a method for producing wood-based yarn filaments from DES-pulp suspension.
- Cellulose plays an important role in textile and filament production.
- the long fibers of natural cotton are ideal for forming strong filaments and yarns, whereby cotton is traditionally utilized in textiles.
- the use of cotton requires lots of water, pesticides and fertilizers in the production phase.
- Wood-based fabrics have been suggested as an ecologically friendly alternative for cotton.
- wood-based cellulose is generally formed as a filament made of dissolved and regenerated cellulose.
- This is also the process that the manmade cellulose-based textile fibres e.g. viscose, modal and lyocell are based on today.
- harmful or toxic chemicals are used, which also have negative effect on the properties of cellulose.
- most of the regenerated cellulose processes are considered unsustainable, and as the crystalline form of cellulose changes in the process, the material properties change drastically as well.
- Short wood fibres do not naturally form strong filaments and they have a tendency to disintegrate in water.
- Ionic solvents have been proposed for dissolving cellulosic materials originating from natural sources. However, they are often harmful or toxic and very expensive for industrial use on a larger scale.
- Deep eutectic solvents are a type of ionic solvents which refer to eutectic mixtures, which melting points are lower than the individual components of separately. Deep eutectic solvents are currently applied in large scale applications, such as electro winning of metals, electro polishing of stainless steel, as well as solvents in organic reactions.
- WO 2012/145522 relates to deep eutectic solvents for the purpose of dissolving cellulose.
- DES-pulp is typically manufactured into the fibre yarn filament by extruding it into ethanol bath.
- the function of the ethanol has been to dissolve the DES away, which requires long time, such as up to 15 minutes.
- NFC fibre yarn filaments have a tendency to stick into the rollers/cylinders in the production process.
- the fiber yarn filament according to an embodiment of the present invention is mainly characterized by what is stated in claim 9 and the use thereof by what is stated in claim 10.
- the present invention provides a simple non-toxic method that uses DES-pulp and laminar solvent flow to produce strong and water- stable fiber yarn filaments.
- the method enables producing more fibre yarn filaments in the same time span as currently has been possible.
- the solvent can be circulated and used again during the production process.
- the present invention reduces the investment costs and the production time and enables easier upscaling of the process.
- the present technology describes a method for manufacturing DES-pulp suspension into a fibre yarn filament.
- the method is continuous.
- Deep eutectic solvents are a sub-class of ionic liquids with special properties. DES is composed of a mixture of two or more components and said mixture forms a eutectic with a melting point much lower than any of the individual components.
- the deep eutectic solvent useful in the present invention consists of hydrogen bond donor and hydrogen bond acceptor.
- FIGURE 1 is a process scheme describing one embodiment of the present invention.
- FIGURE 2 is a process scheme describing another embodiment of the present invention.
- the present invention is based on extruding DES-pulp suspension into flowing solvent.
- the function of the flowing solvent is to dissolve DES from the extruded filament.
- Laminar flow of the solvent immediately starts the dissolution process of DES, providing substantially shortened DES-removal time. In turn, this enables less time consuming method for yarn filament production from such starting material.
- the deep eutectic solvent is selected from the group consisting of DESs, which are able to swell cellulosic material without dissolving it, whereby the cellulosic material can be dispersed in the DES.
- the DESs suitable for the present invention are selected from DESs composed of choline chloride and urea, choline chloride and malonic acid, choline chloride and oxalic acid, choline chloride and phenylacetic acid, and choline chloride and glycerol.
- Choline chloride acts as the hydrogen bond acceptor and the hydrogen bond donor is selected from urea, malonic acid, oxalic acid, phenylacetic acid and glycerol.
- a DES composed of choline chloride and urea is used.
- the DES comprises a molar ratio from 5: 1 to 1 :3, preferably from 3: 1 to 1 :2 of choline chloride and the hydrogen bond donor, respectively. Particularly preferably a molar ratio 1 :2 of choline chloride and the hydrogen bond donor, preferably urea is used. Suitable molar ratio for choline chloride and malonic acid is 1 : 1.
- One embodiment of the present invention is a method for continuously producing wood-based yarn filaments, the method having at least the steps of: suspending a cellulosic material in a DES (deep eutectic solvent) comprising choline chloride and urea at temperature of 10 to 280 °C for obtaining a DES-pulp suspension, and extruding the DES-pulp suspension into a solvent, wherein the DES-pulp suspension is extruded into a running laminar solvent flow at a speed of 1 to 15 cm/s, after which the produced fiber yarn filaments are collected and dried.
- DES deep eutectic solvent
- the method uses a solvent which is an alcohol that is capable to dissolve the components of the used DES.
- the solvent is ethanol.
- suspending a cellulosic material in DES comprising choline chloride and urea is carried out at temperature of 10 to 130 °C for obtaining the desired DES-pulp suspension.
- the laminar solvent flow speed is between 2 and 10 cm s, preferably between 3 and 6 cm/s, such as 4.5 cm/s. It is possible to change the solvent flow speed for example by altering the pumping speed or by changing the angle of the gutter, wherein the extrusion takes place.
- the solvent is recycled back to the process by a pump and used at least two times.
- the cellulosic material may comprise a wide variety of cellulose based raw materials. For example pulp fibres derived from wood pulp may be used.
- mechanically treated pulp fibres such as chemithermomechanical pulp fibres (CTMP), bleached chemithermomechanical pulp fibres (BCTMP), thermomechanical pulp fibres (TMP), refiner groundwood pulp fibres, groundwood pulp fibres, enzymatically treated pulp, cellulose microparticles, cellulose nanoparticles, micro fibrillated cellulose, nanocellulose, enzymatically fibrillated cellulose, and combinations thereof may be used.
- CMP chemithermomechanical pulp fibres
- BCTMP bleached chemithermomechanical pulp fibres
- TMP thermomechanical pulp fibres
- refiner groundwood pulp fibres groundwood pulp fibres
- groundwood pulp fibres enzymatically treated pulp
- cellulose microparticles cellulose nanoparticles
- micro fibrillated cellulose nanocellulose
- enzymatically fibrillated cellulose and combinations thereof
- the cellulosic material is hardwood pulp. This is preferred in order to obtain continuous fibre yarn filaments.
- Thickness of the fiber yarn filament may be changed according to the end-use purpose by altering the nozzle size in the extrusion.
- Single filaments with variable thickness can also be twisted and plied into multifilament yarns with texture depending on the plying technique. Twisting even a single filament improves tenacity values and plying and cabling several filaments improves the values even more.
- Fibre yarn filaments from cellulosic materials is considered as a sustainable alternative for cotton.
- the use of these alternative wood-based raw materials reduces sweet water consumption, particularly for irrigation, as well as occupation of agricultural land and the use of plant protection chemicals.
- a further advantage of the present invention is the recyclability of the DES and solvents used in the process.
- At least some embodiments of the present invention find industrial application among for example yarns, ropes, textiles and cloths.
- the obtained filaments are stable in water.
- the water stable filaments are used as such, but plying them into multifilament yarns and ropes further widens their use.
- textile applications benefit from lightness and possibility for coloured or multicoloured yarn.
- the obtained high quality wood cellulose filaments can be used in wood-based cellulosic fabrics. These fabrics can be used where ever natural fibre fabrics are needed, e.g. clothing, technical textiles etc., thus providing inexpensive and eco- friendly wood-based textiles.
- the high quality wood cellulose filaments are particularly suitable for products which are directly dependent on long fibre filament.
- the DES-pulp solution was prepared as follows. ChCl/urea DES was prepared by mixing ChCl and urea together in a mole ratio of 1 :2, respectively and heated at 100°C with constant stirring until a clear homogenous liquid was formed, followed by drying at 40°C overnight under vacuum, whereby the water content was reduced to less than 1 wt%. Prior to adding in ChCl/urea, the pulp was washed with excess acetone and dried at 40°C overnight under vacuum whereby the water content was reduced to less than 1 wt%. Spinning dopes were prepared by dispersing the pulp in ChCl/urea overnight at 100°C temperature with constant stirring. The dispersions were then cooled and mixed in a Speedmixer under vacuum (800 rpm for 2 min and 1500 rpm for 8 min).
- the DES containing typically 4 % of anhydrous pulp fibres was place into a syringe containing a nozzle with required dimensions.
- the DES-pulp suspension is extruded into a laminar ethanol flow in a canal with downward slope (5-20 degrees).
- the ethanol flow takes the wet filament ribbon from the nozzle and transports the wet filament ribbon into the collection chamber.
- the flow rate of ethanol is above the flow rate of the DES-pulp suspension from the nozzle.
- the difference in the flowrate maintains straight filament direction and can stretch the filament.
- the continuous flow around the filament accelerates the diffusion out of the DES chemicals from the filament.
- the filament After keeping the filament in the collection chamber for 30 to 120 min, the filament is wound and heat activated in an oven at 130 °C for 20 min.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Multicomponent Fibers (AREA)
- Paper (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FI20175927A FI127726B (en) | 2017-10-20 | 2017-10-20 | Method for producing wood-based yarn filaments |
PCT/FI2018/050770 WO2019077208A1 (en) | 2017-10-20 | 2018-10-22 | Method for producing wood-based yarn filaments |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3697950A1 true EP3697950A1 (en) | 2020-08-26 |
Family
ID=64332102
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP18804034.9A Pending EP3697950A1 (en) | 2017-10-20 | 2018-10-22 | Method for producing wood-based yarn filaments |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP3697950A1 (en) |
FI (1) | FI127726B (en) |
WO (1) | WO2019077208A1 (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111384462A (en) * | 2019-12-27 | 2020-07-07 | 中国矿业大学 | Method for preparing graphene by recovering graphite from waste lithium ion battery negative electrode material |
US20230066995A1 (en) * | 2020-02-18 | 2023-03-02 | Aalto University Foundation Sr | A coagulation bath system for fiber spinning |
WO2023034885A1 (en) | 2021-08-31 | 2023-03-09 | Apani Systems Inc. | Textile recycling |
CN114775087B (en) * | 2022-04-29 | 2023-06-23 | 齐鲁工业大学 | Method for improving surface structure of regenerated cellulose fiber |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012145522A2 (en) | 2011-04-19 | 2012-10-26 | Georgia Tech Research Corporation | Deep eutectic solvent systems and methods |
WO2016135385A1 (en) * | 2015-02-27 | 2016-09-01 | Teknologian Tutkimuskeskus Vtt Oy | Process for producing shaped articles based on cellulose |
-
2017
- 2017-10-20 FI FI20175927A patent/FI127726B/en active IP Right Grant
-
2018
- 2018-10-22 WO PCT/FI2018/050770 patent/WO2019077208A1/en unknown
- 2018-10-22 EP EP18804034.9A patent/EP3697950A1/en active Pending
Also Published As
Publication number | Publication date |
---|---|
FI127726B (en) | 2019-01-15 |
WO2019077208A1 (en) | 2019-04-25 |
FI20175927A1 (en) | 2019-01-15 |
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