US3663675A - Process for producing crimped polypropylene filaments - Google Patents
Process for producing crimped polypropylene filaments Download PDFInfo
- Publication number
- US3663675A US3663675A US58207A US3663675DA US3663675A US 3663675 A US3663675 A US 3663675A US 58207 A US58207 A US 58207A US 3663675D A US3663675D A US 3663675DA US 3663675 A US3663675 A US 3663675A
- Authority
- US
- United States
- Prior art keywords
- filaments
- temperature
- crimps
- spinning
- crimped
- 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.)
- Expired - Lifetime
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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
- D01F6/06—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins from polypropylene
Definitions
- the crimped filaments of the invention have extremely fine crimps and have a crimping ability which remains substantially constant if the filaments are relaxed again, even if the filaments are kept under tension for a long time after drawing. Crimped filaments having very little give can be obtained by appropriate selection and regulation of the polypropylene starting material, the spinning conditions, the heat treatment of the undrawn filaments and the temperature at which the filaments are drawn. These conditions must all be maintained within limited ranges in order to obtain the advantages of the invention.
- Crimped polypropylene filaments obtained by the practice of the present invention have a much larger crimping number and a far smaller crimping size in comparison with crimped polypropylene filaments which were previously known. If crimped polypropylene filaments obtained by previously known methods are kept under tension for a long time after the drawing process, for instance, if filaments are kept wound around the drawing pirn for several days, the crimping number decreases in comparison with the crimping number of filaments which are not kept under tension, and sufiicient crimps cannot be obtained even if the filaments are subjected to heat treatment after relaxation all of which results in a failure to obtain good marketable crimped filaments.
- the same extremely fine crimps as those obtained by relaxing immediately after drawing can be obtained within about two minutes.
- sufficiently fine crimps can be obtained, and the degree of fineness of the crimps changes little even if the filaments are subsequently heat treated.
- crystalline polypropylene having an intrinsic viscosity of 1.2 to 2.2 which is obtained by depolymerizing polypropylene having an intrinsic viscosity of 1.2 to 4.2 is used.
- This polymer is melt and pushed out to form pellets for spinning.
- the polypropylene raw material of the present invention must also have a depolymerization degree of less than 1.9, preferably less than 1.5, to be suitable for the spinning operation.
- depolymerization degree is defined as follows:
- Depolymerization degree 1sp/C]P/['71 c]S
- [1 p represents the reduced viscosity of the polymer obtained by the polymerization process
- 1s represents the reduced viscosity of the polymer when it is used as the raw material for spinning.
- the reduced viscosity this value is determined by measuring this viscosity of Tetralin solution of the polymer (0.1 g./ ml.) at C., with an improved model Ostwald viscometer.
- thermal stabilizers such as 2,6-ditert-butyl-p-cresol (0.1 weight percent), light stabilizers such as 2-hydroxy-4-octoxy-benzophenone (0.3 weight percent), stabilizers against gas discoloration, delustering agents such as titanium dioxide, fluorescent bleaching agents, pigments, crystalline nuclei forming agents such as sodium benzoate, and various types of dyeability accelerating agents, such as poly (aminotriazole) (520 weight percent) all of which additives are known in the prior art and have been used in making polypropylene filaments.
- thermal stabilizers such as 2,6-ditert-butyl-p-cresol (0.1 weight percent)
- light stabilizers such as 2-hydroxy-4-octoxy-benzophenone (0.3 weight percent)
- stabilizers against gas discoloration such as titanium dioxide, fluorescent bleaching agents, pigments, crystalline nuclei forming agents such as sodium benzoate
- dyeability accelerating agents such as poly (aminotriazole) (520 weight percent
- the conditions under which the polypropylene is melt spun are very important and must be carefully regulated.
- the spinning temperature should be 260-280 C. at the spinneret. If temperatures of as little as 10 C. higher or lower than this range are employed, fine crimps cannot be obtained even if the other steps of the process are carried out in accordance with the present disclosure.
- the spinneret temperature can be measured simply and accurately by making a small hole in the spinneret surface, and inserting a thermistor through the hole.
- the spinning speed also influences the crimping characteristics of the resulting filaments. Although crimps can be obtained to some extent at a spinning speed of less than 600 m./min., it is necessary to have a spinning speed of more than 600 m./min. to obtain the fine crimps sought by the present inventors.
- the intrinsic viscosity of the pellets before spinning used in the present invention must be 1.2-2.2, but the intrinsic viscosity of the taken-up undrawn filaments thus spun should be 0.8-1.4 to give excellent crimpable filaments.
- the intrinsic viscosity of 0.8-1.4 of the undrawn filaments should be given by just the way by which the pellets are extruded and melt-spun under the conditions as described above. In another words, the intrinsic viscosity of the undrawn filaments ranging from 0.8 to 1.4 may be resulted by from carrying out process under only the conditions that:
- the conditions under which the undrawn filaments are heat treated, and the drawing conditions be carefully regulated. If the heat treatment of the undrawn filaments is either omitted or carried out at a temperature lower than the prescribed range of 120- 150 C., either no crimps are obtained, or the crimps are far inferior to the fine crimps which are the object of the present invention, even if drawing is carried out in the prescribed range of -150 C., and the filaments are thereafter relaxed.
- the heat treatment of the undrawn filaments within the prescribed temperature range apparently has the effect of increasing the potential crimp producing ability of the filaments, as is seen from the fact that crimps can be obtained even if drawing is done at a temperature of 1l0-150 C., although it has heretofore been considered that crimps could not be obtained at such high drawing temperatures. Furthermore, according to the invention, finer crimps can be obtained than those obtainable by drawing at lower temperature filaments which were not subjected to the heat treatment.
- the temperature and the duration of the heat treatment are inversely related, i.e., to achieve the same effect of the heat treatment step, at high temperatures, the duration of the heat treatment may be shorter. For instance, at a temperature of 130 C., a duration of about 30 minutes for the heat treating step will do, but at a temperature of C., more than one hour is required. The duration of the heat treatment will normally vary from about 10 minutes to about 2 hours.
- the draw ratio is not specifically limited but it is normally 1.1-5.0, preferably 2.0-4.0.
- the number of crimps differs according to the denier of the filament. Fine crimps can be obtained according to the present invention with a number of crimps of more than 40 per 25 mm. in the case of single 1-5 (1. filament for clothing, and 25 per 25 mm. even in the case of single 15 d. filament.
- the number of crimps according to the commonly known process is less than a half of that which can be obtained according to the present invention.
- the crimped filaments of the invention have the properties mentioned above, if the drawn filaments are subjected to a knitting process directly from a drawing pirn, the crimp producing speed is fast and crimps can be produced under the tension applied to the filaments at the time of knitting, so that a product similar to knitted goods obtained by knitting ordinary crimped yarns produced by conventional methods can be obtained,
- crimp extension percentage and the crimp recovering percentage which are used in the following examples to show the crimping characteristics of the crimped filaments obtained according to the present invention, are defined as follows:
- EXAMPLE 1 With titanium trichloride and diethyl aluminum chloride used as catalysts and a small amount of hydrogen as a molecular weight modifier, propylene was polymerized in n-hexane, and the resultant polymer was refined to obtain polypropylene in powdery form having a reduced viscosity of 2.0, i.e., an intrinsic viscosity of 1.8, and nheptane content of 2.1%.
- thermo stabilizer 0.1% of 2,6-di-tert-butyl-pcresol was added to this polymer, and this mixture was treated in a pelletizer to obtain a granular polymer having a reduced viscosity of 1.8, i.e., an intrinsic viscosity of 1.65, for use as a spinning raw material.
- the depolymerization degree of this raw material was 1.1.
- melt spinning machine For spinning, an ordinary type of melt spinning machine comprising a combination of an extruder and a gear-pump was used.
- the temperature at the spinneret was 265 C.
- the spinneret had 24 holes, each having a diameter of 0.45 mm.
- the extruded melt filament was cooled down by cold air having a temperature of 20 C.
- the spinning was carried out at atake-up speed of 800 m./min.
- the resultant undrawn filaments were treated for one hour at 140 C., as they were wound around bobbins. These undrawn filaments were drawn by a conventional draw twister. Drawn filaments of 70 d./24 filaments were obtained under the following drawing conditions, i.e., a drawing temperature of 140 C., a draw ratio of 3.0, and a drawing speed of 400 m./min.
- the resultant drawn filaments were made into a hank form, with the result that extremely fine crimps were produced, and they quickly reached an equilibrated status.
- the characteristics of the crimped filaments were as follows:
- Crimp extension percentagel 20% Crimp recovering percentage-91% Number of crimpsS 1/25 mm.
- Crimp extension percentage-l 25 Crimp recovering percentage-93% Number of crimps-5 l 25 mm.
- EXAMPLE 3 To crystalline polypropylene of powdery form having a reduced viscosity of 2.5 i.e., an intrinsic viscosity of 2.2 obtained through polymerization by the same method as in Example 1, there was added 0.2% of 2,6-di-tert-butyl-pcresol as a thermal stabilizer. This mixture was extruded from a pelletizer in granular form, and a polymer having a reduced viscosity of 2.0, i.e., an intrinsic viscosity of 1.8 was obtained. This polymer was used as a raw material for spinning. The depolymerization degree of this polymer was 1.25. The undrawn filaments obtained by spinning this polymer through a spinneret at a temperature of 275 C.
- Crimping elongation-83 Crimping magnification90% Number of crimps-32/ 25 mm.
- EXAMPLE 4 3 kg. of trioctylamiue and 3 kg. of precipitated calcium carbonate having a mean granular diameter of 005g were mixed with 94 kg. of granular polypropylene having an intrinsic viscosity of 1.8 and a depolymerization degree of 1.25 which was obtained by the same method as in Example 3. This mixture was extruded from a pelletizer to obtain a granular polymer. This polymer was subjected to spinning through a spinneret at a temperature set at 265 C. and spinning speed at 900 m./rnin. The resultant filaments were heat treated at 135 C. for 20 minutes.
- the filaments were dyed a reddish orange.
- the characteristics of the resultant crimped filaments were the same as those before dyeing and no yielding was recognized. (This is an example in which the draw ratio was 2.3 times.)
- EXAMPLE 5 Spinning material was prepared by mixing the same crystalline polypropylene as used in Example 1 with 5% of titanium dioxide. The spinning conditions are as follows:
- EXAMPLE 6 To the same polypropylene granules as employed in Example 3 was added 6% by weight of Nylon 6 polymer, 3% by weight of precipitated calcium carbonate having a mean granular diameter of 0.05p. and 8% of liquid paraffin, and the combined materials were mixed well by using a Banbury mixer and then re-pelletized by means of an extruder.
- the resultant undrawn filaments were treated for one hour at 140 C. as they were wound around bobbins.
- Drawn filaments of 70 d./24 filaments were obtained under the following drawing conditions, i.e., a drawing temperature of C., a draw ratio of 3.0, and a drawing speed 300 m./rnin.
- Comparison 1 Isotactic polypropylene having an intrinsic viscosity (in Tetralin at C.) of 3.3 to which 0.4% of an antioxidant and 0.02% of di-butyl tin maleate as a thermal decomposer was fed into a 25 mm. screw-extruder from which the molten polymer was supplied to a metering pump and thence through a filter consisting of 10-20 mesh sand to a two hole spinneret (hole diameter: 0.015 inch). These spinning conditions are shown in Table l. The spun yarns were then cold drawn using a water bath at 90 C. at the required draw ratio and at a draw speed of 200 feet per minute.
- the drawn yarns were then relaxed quickly by cutting the yarn off the draw bobbin and stabilized by heating in air at C. for twenty minutes.
- the Table 1 which follows shows the effect of spinning temperature and wind-up speed on the intrinsic viscosity and birefringence of the spun yarn and the effect of draw ratio on the degree of spontaneous crimping obtained.
- the resultant crimped filament was conspicuously low in degree of crimping as compared with the crimped filament obtained in accordance with the present process. Further, there was unevenness in the degree of crimping of the resultant filament and it may be said that the resultant crimped filament had entirely no commercial value.
- Comparison 2 Extrusions were eifected through a spinneret of 0.015 inch x 2 holes at a spinning temperature of 260 C. and taking-up velocity of 2000 lit/min. varying the extruding amount with the use of the same pellet and device as in Comparison 1. The taken-up filament was immediately heat treated at 140 C. for 30 minutes without drawing. The results are shown in Table 2.
- a process for producing crimped polypropylene filaments comprising melt-spinning crystalline polypropylene having an intrinsic viscosity of 1.2 to 2.2 which is obtained by depolymerizing polypropylene having an intrinsic viscosity of 1.2 to 4.2 by a depolymerization degree of less than 1.9, and at most 20% by weight of additives through a spinneret heated to a temperature of 260 to 280 C., at a spinning speed of more than 600 m./min.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1226867 | 1967-02-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3663675A true US3663675A (en) | 1972-05-16 |
Family
ID=11800604
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US58207A Expired - Lifetime US3663675A (en) | 1967-02-28 | 1970-07-24 | Process for producing crimped polypropylene filaments |
Country Status (5)
Country | Link |
---|---|
US (1) | US3663675A (ja) |
CH (1) | CH485046A (ja) |
DE (1) | DE1710605B1 (ja) |
FR (1) | FR1558655A (ja) |
GB (1) | GB1145818A (ja) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4221838A (en) * | 1972-12-29 | 1980-09-09 | Phillips Petroleum Company | Crimped thermoplastic fibers |
US4384098A (en) * | 1981-01-13 | 1983-05-17 | Phillips Petroleum Company | Filamentary polypropylene and method of making |
US5281378A (en) * | 1990-02-05 | 1994-01-25 | Hercules Incorporated | Process of making high thermal bonding fiber |
US5629080A (en) * | 1992-01-13 | 1997-05-13 | Hercules Incorporated | Thermally bondable fiber for high strength non-woven fabrics |
US5705119A (en) * | 1993-06-24 | 1998-01-06 | Hercules Incorporated | Process of making skin-core high thermal bond strength fiber |
US5882562A (en) * | 1994-12-19 | 1999-03-16 | Fiberco, Inc. | Process for producing fibers for high strength non-woven materials |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AT160896B (de) * | 1927-02-15 | 1943-03-29 | Ig Farbenindustrie Ag | Textilgebilde aus Kondensationspolymeren und Verfahren zu ihrer Herstellung |
AT225836B (de) * | 1959-02-18 | 1963-02-11 | Montedison Spa | Verfahren zur Herstellung eines voluminösen Garnes |
AT229479B (de) * | 1960-08-30 | 1963-09-25 | Rhodiaceta | Verfahren zur Herstellung von Kräuselfäden |
BE628987A (ja) * | 1962-02-27 | |||
FR1353724A (fr) * | 1963-02-27 | 1964-02-28 | Ici Ltd | Procédé de fabrication de fibres ou filaments en polypropylène isotactique |
-
1968
- 1968-02-27 GB GB9505/68A patent/GB1145818A/en not_active Expired
- 1968-02-27 FR FR1558655D patent/FR1558655A/fr not_active Expired
- 1968-02-27 DE DE19681710605 patent/DE1710605B1/de not_active Withdrawn
- 1968-02-27 CH CH283068A patent/CH485046A/fr not_active IP Right Cessation
-
1970
- 1970-07-24 US US58207A patent/US3663675A/en not_active Expired - Lifetime
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4221838A (en) * | 1972-12-29 | 1980-09-09 | Phillips Petroleum Company | Crimped thermoplastic fibers |
US4384098A (en) * | 1981-01-13 | 1983-05-17 | Phillips Petroleum Company | Filamentary polypropylene and method of making |
US5281378A (en) * | 1990-02-05 | 1994-01-25 | Hercules Incorporated | Process of making high thermal bonding fiber |
US5318735A (en) * | 1990-02-05 | 1994-06-07 | Hercules Incorporated | Process of making high thermal bonding strength fiber |
US5431994A (en) * | 1990-02-05 | 1995-07-11 | Hercules Incorporated | High thermal strength bonding fiber |
US5629080A (en) * | 1992-01-13 | 1997-05-13 | Hercules Incorporated | Thermally bondable fiber for high strength non-woven fabrics |
US5654088A (en) * | 1992-01-13 | 1997-08-05 | Hercules Incorporated | Thermally bondable fiber for high strength non-woven fabrics |
US5733646A (en) * | 1992-01-13 | 1998-03-31 | Hercules Incorporated | Thermally bondable fiber for high strength non-woven fabrics |
US5888438A (en) * | 1992-01-13 | 1999-03-30 | Hercules Incorporated | Thermally bondable fiber for high strength non-woven fabrics |
US5705119A (en) * | 1993-06-24 | 1998-01-06 | Hercules Incorporated | Process of making skin-core high thermal bond strength fiber |
US6116883A (en) * | 1993-06-24 | 2000-09-12 | Fiberco, Inc. | Melt spin system for producing skin-core high thermal bond strength fibers |
US5882562A (en) * | 1994-12-19 | 1999-03-16 | Fiberco, Inc. | Process for producing fibers for high strength non-woven materials |
Also Published As
Publication number | Publication date |
---|---|
GB1145818A (en) | 1969-03-19 |
DE1710605B1 (de) | 1971-04-01 |
CH485046A (fr) | 1970-01-31 |
FR1558655A (ja) | 1969-02-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US4163770A (en) | Melt-spinning acrylonitrile polymer fibers | |
US3038235A (en) | Textile fibers and their manufacture | |
US2604667A (en) | Yarn process | |
EP0213208B1 (en) | Polyethylene multifilament yarn | |
US4863664A (en) | High speed process of making polyamide filaments | |
US3663675A (en) | Process for producing crimped polypropylene filaments | |
EP0042664B1 (en) | Polyester yarns produced by high speed melt-spinning processes | |
US3655857A (en) | Process for preparing acrylonitrile polymer solution | |
US4113821A (en) | Process for preparing high strength polyamide and polyester filamentary yarn | |
US3523150A (en) | Manufacture of industrial acrylic fibers | |
US3088793A (en) | Spinning of acrylonitrile polymers | |
US2385890A (en) | Spinning process | |
US3054652A (en) | Isotactic polypropylene melt spinning process | |
US3641760A (en) | Foam fibrillated yarn and process | |
US5993712A (en) | Process for the processing of polymer mixtures into filaments | |
JPH026613A (ja) | ポリスチレンを含む伝導性フィラメント,その製造方法,多フィラメント系及びカーペット | |
US3080210A (en) | Spinning of acrylonitrile polymers | |
JP2003301327A (ja) | 耐加水分解性に優れたポリ乳酸繊維 | |
EP0346641A2 (de) | Verfahren zur Herstellung gleichmässiger POY-Filamente | |
CA1233009A (en) | High speed process for forming fully drawn polyester yarn | |
DE4320593A1 (de) | Multifilament-Garn aus Polyäthylennaphthalat und Verfahren zu seiner Herstellung | |
US2924503A (en) | Process for melt spinning polyesters containing an alkaline earth sulfate filler | |
US3539676A (en) | Process for producing filaments and films of polymers of alkylene sulfides | |
US2721785A (en) | Acrylonitrile-styrene copolymer filaments and process of producing same | |
US3808302A (en) | Process for producing low-pilling textile fiber |