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WO2001086042A1 - Procede de preparation d'un produit façonne en cellulose - Google Patents

Procede de preparation d'un produit façonne en cellulose Download PDF

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Publication number
WO2001086042A1
WO2001086042A1 PCT/JP2001/003884 JP0103884W WO0186042A1 WO 2001086042 A1 WO2001086042 A1 WO 2001086042A1 JP 0103884 W JP0103884 W JP 0103884W WO 0186042 A1 WO0186042 A1 WO 0186042A1
Authority
WO
WIPO (PCT)
Prior art keywords
cellulose
dope
pulp
water
chemical
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.)
Ceased
Application number
PCT/JP2001/003884
Other languages
English (en)
Japanese (ja)
Inventor
Kazutake Okamoto
Yasuo Ohta
Yoshihiko Teramoto
Muneatsu Nakamura
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyobo Co Ltd
Original Assignee
Toyobo Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from JP2000136840A external-priority patent/JP2001316938A/ja
Priority claimed from JP2000136839A external-priority patent/JP2001316937A/ja
Application filed by Toyobo Co Ltd filed Critical Toyobo Co Ltd
Publication of WO2001086042A1 publication Critical patent/WO2001086042A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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 technique for forming a cellulose raw material into ⁇ with a solvent such as tertiary amine oxide and forming the fiber into a fiber, rod, sheet, or membrane. ⁇ J3 ⁇ 4 technology
  • NMMO N-methylmorpholine mono-N-oxide
  • NMMO is a type of tertiary amoxide and is an organic solvent. Using this solvent, it is possible that used cloth, annual grass, etc. can be converted to
  • the a-cellulose content is 90, which is derived from wood such as softwood and hardwood.
  • Chemical pulp refined to have a ratio of / 0 or more is used industrially. This chemical pulp has a controlled degree of cellulose polymerization and components, and is safe without breaking even in a molding method that has a process of stretching thinly, such as a sensitive film. It is possible to produce in a fixed manner.
  • ⁇ ⁇ is usually reused as paper after the purified panoleb is added to paper once and used. However, there are some factors that are not reused as paper due to various factors, and effective utilization is desired. Disclosure of the invention
  • the present invention employs the following means to solve the above problem.
  • the first embodiment of the present invention relates to a method of controlling the morphology by discharging cellulose tertiary amine oxide containing 1% by weight or more of chemical pulp and waste paper or Z and kenaf, followed by coagulation and dissolution. This is a method for producing a characteristic cellulose molded article.
  • the cell according to the above item 1 wherein the chemical pulp and the pulp or Z and kenaf are individually dissolved in tertiary amine oxide, and each cellulose solution is mixed in a molding step. This is a method for producing a mouth-formed body.
  • the third embodiment of the present invention is the method for producing a cellulose molded article according to item 1, wherein the above-mentioned cellulose solutions are discharged in a composite manner from an extrusion die.
  • a fourth embodiment of the present invention is a cell mouth molded product, characterized in that the outermost layer is S chemical pulp cellulose and the inner layer is waste paper or cellulose containing napkin and kenaf pulp.
  • the chemical pulp in the present invention is a pulp that has been subjected to delignification treatment, which is generally called chemi-canole pulp, and examples thereof include sulfite pulp, sulfate pulp, and soda pulp.
  • the mixing ratio of the chemical pulp with Mr. Z or Z and kenaf is such that the ratio of the chemical pulp is 1% by weight or more. If the amount of controlled chemical pulp is less than 1%, the effect of improving poor moldability of waste paper or dope only with Z and kenaf is small.
  • the percentage of chemical pulp should be as small as possible from the viewpoint of the use of pulp or kenaf, usually 90% by weight. The following degree is desirable.
  • a cellulose molded article of stable quality can be produced.
  • one chemical pulp component is 5 weight.
  • the above is preferable for stable co-extrusion. It is preferable that the degree of polymerization of the chemical panolep used is appropriately selected according to the quality of the waste paper / kenaf pulp to be combined. If the degree of polymerization of kenaf pulp is high, it is also possible to use a combination in which the degree of polymerization of iridani pulp is lower than that. It's preferable.
  • Aminoxide in the present invention is an organic solvent capable of dissolving cellulose typified by di-methylmorpholine mono-oxide at a concentration of 10% by weight or more.
  • This finished minoxide may contain an antioxidant, a ⁇ adjuster, and a third component for adjusting the fluid characteristics of the solvent.
  • a tertiary amine oxide solution of cellulose is discharged from a spinneret for producing fibers, a slit die for producing films, a mold gate, or the like, and is subjected to uniaxial stretching, blow stretching, and foaming.
  • the form of the ejected material is controlled by molding.
  • the present invention is not limited to the above-described example with respect to the method of controlling the shape of the ejection intense night, and can select a molding method suitable for a desired molded product.
  • the morphology is fixed by contact with a non-solvent to solidify.
  • a non-solvent used here, water, lower alcohols, ketones such as acetone can be used, but water is preferable when industrially large amounts are used.
  • the solvent in the compact is extracted.
  • non-solvent water or the like can be used, but a supercritical fluid may be used.
  • the above-mentioned molded body may be used as a porous body containing a solvent, but when used as an concealed film, a drying step for removing the ⁇ medium in the molded body is necessary. Drying can be performed by any method such as heating with hot air, air drying at room temperature, and freeze drying. It is also possible to crimp the flakes before or after drying, cut and use them, or cut the film into a tape shape and use it as flat yarn. Before or after processing molded articles into knitted or woven fabrics, dyeing or kneading, surface treatment or modification It is also possible to apply processing.
  • Japanese paper made from kozo, mitsumata, and ganpi hemp is preferred because it is easier to wash inorganic substances than paper, and has a higher utility value than recycled paper A ⁇ ii.
  • two or more kinds of cellulose raw materials can be used.
  • the dissolution rate varies depending on the cellulose raw material. Therefore, it is necessary to adjust the grinding conditions and dissolution time of the raw material accordingly. Also, the conditions for filtering foreign substances in the raw material need to be changed according to the amount and size of the foreign substances contained. Therefore, it is preferred that chemical pulp and ⁇ ⁇ ⁇ or Z and kenaf pulp be separately put into a melting facility.
  • This method has the advantage of mixing the dissolved cellulose dope with a liquid or extruding the cellulose dope individually to form a composite.
  • it is difficult to uniformly disperse and mix a plurality of celluloses in the state of the pulverized cell mouth, but in a liquid state, uniform mixing can be achieved by appropriately using a mixing device.
  • a means for uniform mixing use a kneader ⁇ twin-screw extruder, single-screw extruder with a mixing mechanism, or a vertical stirring can in the undissolved or semi-dissolved slurry state or completely dissolved state. Can be.
  • the clearance of the stirrer is small, and a device capable of mixing with a high degree of spiral is preferred.
  • individual dissolution is essential.
  • Waste paper and / or kenaf nolp can be bleached, but not always as well as chemical pulp. It is also possible to use unbleached materials in terms of environmental distribution and raw material costs. In this way, by performing composite molding, unbleached ⁇ or Z and kenaf can be arranged on the core, and chemical pulp can be arranged on the outer periphery or on the surface (outermost layer), thereby improving the design. Become.
  • the molded article according to the present invention described above is used as a material for clothing, a packaging material, and an industrial material.
  • the measuring method used in the present invention is as follows.
  • the degree of polymerization of cellulose was measured by the Kyupri-Ethylenediamine method ("Polymer Material Testing Method 2", edited by The Society of Polymer Science, Japan, Kyoritsu Shuppan, 1967). The sample was weighed from 0.075 to 0.085 g and placed in a solution of Kiupuri's ethylenediamine. After stirring at room temperature for about 30 minutes to completely dissolve the sample, the viscosity was measured using a Ube-Mouth Ide-Psychometer, and the degree of polymerization was determined.
  • the moisture content in the dope was measured with a trace moisture measuring device (Hiranuma Sanyo Shikikai, Model AQ-7). About 1 g of the test piece was weighed, about 10 ml of absolute ethanol (99.5%) was added, and the mixture was allowed to stand at room temperature and then measured.
  • a trace moisture measuring device Hiranuma Sanyo Shikikai, Model AQ-7.
  • the water content in this dope was 11.2%. Both of these two dopes were amber-colored viscous materials. Each dope of the chemical cellulose and the fc paper was coagulated and precipitated, washed with water, and dried, and the degree of polymerization of each cellulose was 600 and 400, respectively.
  • Each of these dopes was filled into two plunger type feed tanks equipped with pistons.
  • the dope supplied from these was measured and supplied through separate gear pumps so that the weight ratio was 75% of waste paper dope and the chemical cellulose dope was 25.
  • the diameter was 3.2 mm and 18 elements.
  • a spinneret having 10 holes and an outlet diameter of 200 ⁇ was used, and the total dope discharge rate was 6.7 g / min.
  • the temperature of the spinneret is 108 ° C, and the wind speed just below it
  • the yarn was cooled with air adjusted to 15 ° C in 1.2 mZ seconds. After water was removed from the nozzle by a coagulation funnel with a depth of 5 Omm 300 mm below the nozzle, the film was wound on a Nelson-type nozzle with water dripped. Nelson roller speed is 4
  • the thickness of «t after air drying at 5 OmZ was 23.3 dtex.
  • Table 1 shows the physical properties of the obtained ft fresh cellulose 3 ⁇ 4i. It has similar mechanical properties as tzrn obtained from chemical cellulose.
  • Example 2 Chemical cellulose 6 0 4 g and 5 0 wt 0 / NMMO solvent 5 6 0 containing water of 0 0 g with stirring with 1 1 0 ° was heated to C and depressurization regulating the cellulose concentration of 1 6% doped It was adjusted. The water content in the dope was 9.8%.
  • paper copied high-quality paper
  • Each of these dopes was filled into two plunger type feed tanks equipped with pistons.
  • the dope supplied from these was metered through individual gear pumps into a sheath core type spinneret with chemical cellulose as a sheath, and ⁇ came to the core.
  • the weight ratio of the discharge amount was 65 for the waste paper dope and 35 for the sheath component dope.
  • the total dope discharge rate was 6.7 g / min.
  • the temperature of the spinneret was set at 108 ° C, and immediately below the spinneret, the air was adjusted to 15 at a wind speed of 1.2 seconds and the yarn was drawn.
  • Table 1 shows the physical properties of the obtained regenerated cellulose Marina Obtained from chemical cellulose
  • Example 2 Only the single dope obtained from (2) in Example 2 was charged into a plunger-type supply tank equipped with biston. The supplied dope was measured and supplied to a spinneret through a gear pump. Using a spinneret having 10 holes and an outlet diameter of 200 m, the total drop discharge rate was 5.2 g / min. The spinneret was set at 105, and the yarn was cooled with air adjusted to 15 at a wind speed of 1.2 mZ seconds immediately below. 30 Omm below the nozzle, brought into contact with water with a 5 Omm deep coagulation funnel, and then water was dropped It was run on the Nelson-type roller and then wound up. The speed of the Nelson roller was 350111 minutes, and the thickness of ⁇
  • the spinneret is a 112 D C, immediately below the cooled the yarn at wind speeds 1. was adjusted to 1 5 2 m / sec air. After being mixed with water using a coagulation funnel having a depth of 5 Omm, which was formed 30 Omm below the nozzle, the mixture was wound on a tunnel-type roller on which water was dropped. The speed of Nelson Roller was 50 Om / min and was air-dried! The thickness of 3 ⁇ 4 ⁇ was 18. Od tex.
  • Table 1 shows the physical properties of the regenerated cellulose obtained. It has the same mechanical properties as those obtained from chemical cellulose.
  • Each of these dopes was filled into two complete plunger supply tanks with bistons.
  • the dope supplied from these was metered through individual gear pumps into a sheath core type spinneret so that the chemical cell mouth dope came to the sheath and the waste paper dope came to the core.
  • the weight ratio of the ejection amount was 70 for the core waste paper dope and 30 for the sheath component dope.
  • a spinneret having an exit diameter of 200 ⁇ with a sea core type of 10 holes was used, and the total dope discharge rate was 6.7 g / min.
  • the spinneret was set at 108 ⁇ , and immediately below it, the yarn was cooled with air adjusted to 15 at a wind speed of 1.2 mZ seconds.
  • the sample After being brought into contact with water through a coagulation funnel having a depth of 30 mm below the nozzle and having a depth of 5 mm, the sample was run on a Nelson roller to which water had been dropped, and wound up. The speed of the Nelson roller was 45 5 ⁇ minutes, and the thickness of »after air drying was 23.6 dtex. As in this example, it is possible to confine the cellulose component derived from waste paper inside the molded article.
  • Chemical cellulose (pulp) 5 6 5 g and 5 0 wt 0/0 with stirring and NMMO solvent 5 6 0 0 g containing water was heated to 1 1 0 ° C ⁇ engineered cellulose concentration of 1 5% of The dope was adjusted. The moisture content in the dove was 10.7%. Further, the kenaf whole stem kraft pulp was heated and ground to 110 with 500 g of powder obtained by crushing and pulverizing the powder and 500,000 g of NMMO solvent containing 50% by weight of water. (4) The operation was adjusted to a dope with a cell opening concentration of 16%. The water content in this dope was 11.2%. Both of these two dopes were amber-colored viscous materials. The individual dopes of chemical cellulose and kenaf pulp were coagulated, precipitated, washed and dried with water, and the degree of polymerization of each cellulose obtained was 600 and 420, respectively.
  • Each of these dopes was filled into two plunger-type supply tanks equipped with bistons.
  • the dope supplied from these was metered through individual gear pumps so that the weight ratio of chemical cellulose dope to kenaf pulp dope 5 was 25 to 25, and the diameter was 3.2 mm, 1
  • the mixture was mixed using a Kenix-type static mixer composed of eight elements and discharged from the spinneret.
  • the spinneret has an exit diameter of 100 holes and a diameter of 200 ⁇ .
  • the discharge rate was 6.7 g / min.
  • the diameter of the spinneret was set at 108 mm, and the air flow was adjusted to 15 at a wind speed of 1.2 m / sec and the yarn was cooled with the air.
  • the film After being brought into contact with water with a coagulation funnel having a depth of 300 mm below the nozzle and having a depth of 5 Omm, the film was wound on a Nelson roller to which water had been dropped.
  • the 53 ⁇ 43 ⁇ 4 of the Nelson roller was 450 m / min and the thickness of the ⁇ after air drying was 23.3 dte X.
  • Table 2 shows the physical properties of the obtained regenerated cell openings. It has mechanical properties comparable to those obtained from chemical cellulose.
  • Chemical cellulose 6 0 4 g and 5 0 wt 0/6 1 with stirring and NMMO solvent 5 6 0 0 g containing water of 1 0 ° was heated in C operate tone cellulose concentration of 1 6% doped integer and did.
  • the water content in the dope was 9.8%.
  • the kenaf core kraft pulp was subjected to force crushing and powdered 529 g and NMMO solvent 560 g containing 50% by weight of water were heated to 110 with stirring and decompressed. An operation was performed to adjust a dope having a cellulose concentration of 1.4%.
  • the water content in this dope was 11.9%. Both of these two dopes were amber-colored viscous materials.
  • the weight of each cellulose obtained by coagulating sedimentation washing and drying of chemical warfare dope of the chemical cellulose and the kenaf core pulp with water was 660 and 320, respectively.
  • Each of these dopes was filled into two plunger-type supply tanks equipped with bistons.
  • the dope supplied from these is passed through individual gear pumps
  • the chemical cellulose was sheathed into the spinneret and the kenaf core pulp was metered into the core.
  • the weight ratio of the ejection amount was 65 for kenaf dope and 35 for sheath component dope.
  • the total dope discharge rate was 6.7 g / "min.
  • the spinneret temperature was 108: Immediately below, the yarn was cooled with air adjusted to 15 ° C at a wind speed of 1.2 mZ seconds and brought into contact with water with a 50 mm deep coagulation funnel 300 mm below the nozzle. Thereafter, the film was wound on a Nelson roller on which water was dropped, and the speed of the Nelson roller was 45 O mZ, and the thickness of »after air-drying was 23.4 dtex.
  • Table 2 shows the physical properties of the product. It has the same mechanical properties as »obtained from chemical cellulose.
  • Example 5 Only the dope obtained from the kenaf core of Example 5 was charged into a plunger type supply tank equipped with a piston. The supplied dope was metered through a gear pump to a new yarn die. Using a spinneret having 10 holes and an outlet diameter of 200 / zm, the total dope discharge rate was 5.2 g / min. The temperature of the spinneret was 105 ° C, and the yarn was cooled with air adjusted to 15 at a wind speed of 1.2 m / sec immediately below. After being brought into contact with water by a coagulation funnel having a depth of 30 mm below the nozzle and having a depth of 5 mm, it was wound on a Nelson roller to which water had been dropped. The speed of the Nelson roller was 350 ⁇ minutes, and the thickness of the note after air drying was 23.1 dteX. Table 2 shows the physical properties of the obtained regenerated / rerose fibers.
  • dopes were filled into two plunger-type supply tanks each equipped with Biston II.
  • the dope supplied from these was metered into a sheath-core type spinneret through individual gear pumps so that the chemical cellulose dough came to the core, kenafno, and rupe dope to the core.
  • the ratio of the sheath component dope to the dope was 70, and the ratio of the sheath component dope was 30.
  • the total drop discharge amount was 6.7 gZ min.
  • the temperature of the spinneret was set to 108, and the yarn was cooled with air adjusted to 15 at a wind speed of 1.2 ⁇ / sec immediately below it, at a depth of 50 mm 300 mm below the nozzle. After contact with water in the coagulation funnel of No. 1, it was run on a Nelson roller on which water was dropped and wound up. It was 3 dtex, as shown in this example. It is possible to confine the loin content inside the molded body.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

L'invention concerne un procédé de préparation d'un produit façonné en cellulose, qui consiste à utiliser une solution de cellulose dans un oxyde d'amine tertiaire, contenant des vieux papiers et/ou de la pâte de kénaf et au moins 1 % en poids d'une pâte chimique, à ajuster la forme de cette solution, puis à la coaguler ou à la soumettre à une extraction avec un solvant. L'invention concerne également un procédé de préparation d'un produit façonné en cellulose, qui consiste à dissoudre la pâte chimique et les vieux papiers et/ou la pâte kénaf séparément, à acheminer ces solutions séparées à un orifice d'extrusion, et à délivrer le mélange obtenu à partir de ce dernier. L'invention concerne en outre un produit façonné en cellulose produit par l'un des procédés susmentionnés. Ce produit façonné en cellulose présente une qualité stable bien qu'il contienne principalement des matières premières de cellulose recyclées et possède ainsi une qualité suffisante pour un usage industriel.
PCT/JP2001/003884 2000-05-10 2001-05-10 Procede de preparation d'un produit façonne en cellulose Ceased WO2001086042A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2000-136839 2000-05-10
JP2000136840A JP2001316938A (ja) 2000-05-10 2000-05-10 セルロース成形体の製造方法
JP2000-136840 2000-05-10
JP2000136839A JP2001316937A (ja) 2000-05-10 2000-05-10 セルロース成形体の製造方法

Publications (1)

Publication Number Publication Date
WO2001086042A1 true WO2001086042A1 (fr) 2001-11-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2001/003884 Ceased WO2001086042A1 (fr) 2000-05-10 2001-05-10 Procede de preparation d'un produit façonne en cellulose

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210054567A1 (en) * 2013-04-17 2021-02-25 Evrnu, Spc Methods and systems for forming composite fibers
US12319790B2 (en) 2013-04-17 2025-06-03 Evrnu, Spc Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55118928A (en) * 1979-03-02 1980-09-12 Akzona Inc Cellulose molded article and its manufacture
JPH09505119A (ja) * 1994-09-05 1997-05-20 レンツィング アクチェンゲゼルシャフト セルロース成形体の製造方法
JPH10331027A (ja) * 1997-05-29 1998-12-15 Toyobo Co Ltd 再生セルロース繊維及びその製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55118928A (en) * 1979-03-02 1980-09-12 Akzona Inc Cellulose molded article and its manufacture
JPH09505119A (ja) * 1994-09-05 1997-05-20 レンツィング アクチェンゲゼルシャフト セルロース成形体の製造方法
JPH10331027A (ja) * 1997-05-29 1998-12-15 Toyobo Co Ltd 再生セルロース繊維及びその製造方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210054567A1 (en) * 2013-04-17 2021-02-25 Evrnu, Spc Methods and systems for forming composite fibers
US12281441B2 (en) * 2013-04-17 2025-04-22 Evrnu, Spc Methods and systems for forming composite fibers
US12319790B2 (en) 2013-04-17 2025-06-03 Evrnu, Spc Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers

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