CN1027982C - Preparing process of fine denier and ultra-fine denier polypropylene fibre P - Google Patents
Preparing process of fine denier and ultra-fine denier polypropylene fibre P Download PDFInfo
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- CN1027982C CN1027982C CN 91104649 CN91104649A CN1027982C CN 1027982 C CN1027982 C CN 1027982C CN 91104649 CN91104649 CN 91104649 CN 91104649 A CN91104649 A CN 91104649A CN 1027982 C CN1027982 C CN 1027982C
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- dawn
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Abstract
The present invention relates to thin denier polypropylene fiber, super thin denier polypropylene fiber and manufacture technique thereof. Spinning technique is stabilized through various measures. When spinning temperature is controlled from 200 to 280 DEG C, the thin denier polypropylene fiber and the super thin denier polypropylene fiber with the monofilament fineness of 0.2 to 2 deniers, the tensile strength of 4 to 8 grams/denier and the breaking elongation rate of 15 to 70 % can be made of high fluidity polypropylene with good heat stability in a mode that fiber is spun at the spinning speed of less than 2000 meters/minute, is wound into silk and is drawn in multiple times. The polypropylene resin for spinning a fine denier filament can be chemical degradation resin with narrow molecular weight distribution (Q<1.3) and a polypropylene resin composition with quite wide molecular weight distribution (the molecular weight distribution index is from 1.3 to 4.0).
Description
The present invention is the manufacture method that belongs to polypropylene fibre.
The invention relates to the manufacturing technology of fine denier polypropylene fibers and superfine denier polypropylene fibers.
Usually, filament number is that chemical fibre about 1 dawn is fine count fiber and filament number is a chemical fibre about 0.5 dawn is called superfine Denier fibre.This fibrid can be made into high-grade textiles soft, comfortable and easy to wear, and very high economic worth is arranged.Thereby the exploitation of fine count fiber and superfine Denier fibre manufacturing technology is the new and high technology all paid attention to of each state in recent years.
The diameter of fine count fiber and superfine Denier fibre is much thinner than conventional chemical fiber (filament number is generally 3-6 about the dawn), the technical difficulty of making this class chemical fibre is quite big-need select appropriate spinning material and auxiliary agent for use, also need technical scheme and every production processes such as strict control spinning, drawing-off of choose reasonable spinning.In recent years, the fine count fiber manufacturing technology of the big kinds of chemical fibre such as polyester fiber and polyamide fiber has been succeeded in developing, and existing many trade names fine-denier polyesters in various countries and thin denier polyamide fiber are sold.Among the manufacturing technology of fine denier polypropylene fibers is also being developed successively.From disclosed patent report in the last few years as can be seen, the technology path of various countries' exploitation fine-denier polypropylene and the specification of product have nothing in common with each other, and its common characteristic is all to adopt the PP Pipe Compound of the quite high acrylic resin of melt flow index as spinning.Some patents claim that the resin dedicated melt flow index of spinning fine denier filament needs to measure according to ASTM D-1238 method up to 300-500(, 230 ℃, 2.16kg).Some patents are said and can be spun into fine count fiber with quite high spinning speed by the chemical degradation of polypropylene resin that this class specification is special, other patents say that then the acrylic resin that melt flow index is very high can be spun into the thinner nonwoven fabric of fibre diameter (rib field etc., JK, 1984,59-94610; Qian Ze etc., JK, 1985,60-17111; Ikeda etc., JK, 1988,63-6107; Shinji storehouse etc., JK, 1988,63-256714).It seems from the trend of the external new trade mark of releasing in recent years of fiber-grade pp resin and some above-mentioned patent reports, many people think, make thin dawn and superfine denier polypropylene fibers and require its material resin that good fluidity of molten, lower molecular weight and narrow molecular weight distribution (Mw/ Mn＜4) are arranged.In addition, also also have indivedual patents to say, the polypropylene of different molecular weight is mixed by a certain percentage can be used for making polypropylene fibre (R.L.Hudson, 1981, USP 4,296,022).The technology of in these patent reports, making good thin dawn of mechanical property and superfine denier polypropylene fibers with conventional melt spinning and draft apparatus and come spinning effect preferably still to lack about acrylic resin and report with which kind of specification about how.Therefore, the manufacturing technology of thin dawn and superfine denier polypropylene fibers needs further exploitation.
The objective of the invention is to develop the fine-denier polypropylene fiber and the spinning new technology of superfine Denier fibre and the thin dawn and the superfine denier polypropylene fibers of good mechanical performance that are applicable to the existing general apparatus for melt spinning of China.A large amount of spinning result of experiment show, many commodity acrylic resins or because of its impurity content more, fluidity of molten is poor, or, all can not satisfy " stably spin thin dawn undrawn yarn and successfully its drawing-off is become the finished fiber of good mechanical performance " these two basic demands because of the problem of aspects such as its molecular weight, molecular weight distribution, isotacticity.In general, spin the fine-denier polypropylene fiber with the isotactic polypropylene resin of polymer grade, its spinnability is relatively poor.Even (Mw/ Mn is about about 4-4.5) that the molecular weight distribution that makes with the carrier model effective catalyst is rather narrow, (about the 16-17 ten thousand) that molecular weight is less, the also goodish fibre resin of fluidity of molten comes spinning, also be difficult to successfully be spun into the high-quality fine denier polypropylene fibers, because if this resinoid spinning temperature is controlled at polypropylene to be taken place below the temperature of degraded (spinning temperature need be controlled at below 270-280 ℃), then spun undrawn yarn is difficult to drawing-off, can't make the fine count fiber of good mechanical performance, if and spinning temperature is elevated to more than 270-280 ℃, then polypropylene degraded rapidly in spinning process, the uniformity of restive fine denier polypropylene fibers spinning process and long-time stability.
Nearly decades, obtained remarkable progress though the macromolecule of various trait is carried out blending and modifying with the research of making various macromolecule new materials, same a kind of macromolecule of different size has been carried out blending and modifying and develop the way of macromolecule new material and as if also do not cause enough attention.The polypropylene of different size is carried out spinning properties and serviceability that can blend improve polypropylene fibre unified understanding is not arranged so far yet.
We recognize in the manufacturing technology process of exploitation fine-denier polypropylene and superfine Denier fibre, spin fine count fiber or superfine Denier fibre with the polymer grade polypropylene resin of various catalyst manufacturing, and its spinnability all can not be satisfactory.Though the polymer grade polypropylene of conventional catalyst manufacturing is carried out that modification is handled and the high-flowability polypropylene resin made can improve the spinnability of its spinning fine denier filament with the control chemical degradation method, but effect still not ideal enough (it may be noted that many now discloseder use this class acrylic resin often as spinning material) about fine denier polypropylene The Study of Manufacturing Technology report.By a large amount of contrast experiments, we find, the polymer grade polypropylene resin made from the carrier model effective catalyst is handled through the chemical degradation modification, and the resin that the melt flow index of making is higher and molecular weight distribution is narrower has preferably spinning properties than preceding two kinds of acrylic resins, and (MI of this resin is about 40, and molecular weight distributing index Q is 1.1-1.5, the Q value is pressed the method for suggestions such as Zhao Delu and is measured, the macromolecule communication, (3), 234,1983).And the spinning properties of the quite wide polypropylene resin composite of molecular weight that polymer grade polypropylene and chemical degradation polypropylene are mixed with and molecular weight distribution excursion also is good.On the basis of a large amount of spinning contrast tests, we have invented the stable spinning new technology that is suitable for making thin dawn and superfine denier polypropylene fibers.
Basic design of the present invention and major technique are constructed as follows:
The objective of the invention is provides a kind of spinning effect good stable spinning new technology at the technical difficulty in fine-denier polypropylene fiber and the superfine Denier fibre manufacturing, and the thin dawn and the superfine denier polypropylene fibers goods that make in this way.It is characterized in that managing to reduce the fluctuation of various technological parameters in the spinning process, suppress the destabilizing factor in the polypropylene fibre manufacture process as much as possible, make the super drawing process of spinning melt and thin dawn undrawn yarn be able to continuously carry out smoothly.For suppress polypropylene in spinning process degraded and cause the inhomogeneities of melt viscosity and acrylic resin can fully be melted when the spinning evenly, polyacrylic melt temperature should be controlled at below 280 ℃ and more than 200 ℃, be preferably between 260 ℃ and 220 ℃ during spinning.Selected acrylic resin should have good heat endurance, promptly need to add the stabilizing agent of q.s and do not contain degradation of promoter in acrylic resin, the inhibition melt polypropylene produces too much thermal degradation in spinning process and chemical degradation causes spinning process to be difficult to stable carrying out.Selected acrylic resin also should have goodish fluidity of molten and tensility, and its melt flow index should be controlled between the 12-100.The acrylic resin of this high fluidity can be the chemical degradation of polypropylene resin of narrow molecular weight distribution, the scope of its molecular weight distributing index Q value is 1.2-1.8, but should select for use quality evenly and the few polymer grade polypropylene of solid impurity as the raw material of chemical degradation modification.The acrylic resin PP Pipe Compound of promptly spinning fine count fiber needs with the chemical degradation agent polymer grade polypropylene of carrier model effective catalyst manufacturing to be carried out control degradation and makes.But, also can be good and the spinning PP Pipe Compound of fine count fiber and superfine Denier fibre is spun in polypropylene resin composite (control range of melt flow index is between 12-100, and the control range of molecular weight distributing index Q value is between 1.3-4.0) conduct that molecular weight distribution is quite wide with fluidity of molten.
It is painted that polypropylene fibre adopts the original liquid coloring method to carry out usually, and used colouring agent normally mixes acrylic resin with the form of Masterbatch and carries out spinning during spinning.When making fine-denier polypropylene fiber and superfine fibre, also can do like this, but preferably select the Masterbatch that is suitable for, it and acrylic resin be mixed even, and carry out mixing granulation, make uniform coloured section.Can reduce the aberration of fine-denier polypropylene fiber and superfine fibre and improve its spinning, drawing-off performance with coloured slice spinning.
The present invention is the stable spinning technique that is applicable to general apparatus for melt spinning.The scope of selected wire winding speed be 300-1500 rice/minute, the hot drawing temperature scope of undrawn yarn is 50-160 ℃.The hot drawing-off of undrawn yarn needs according to the condition of the selected raw material of spinning, spinning and the requirement of finished fiber is decided, and drafting multiple generally can be controlled between 2.5-6 times, is preferably about 3-4 times.
Can be spun into the undrawn yarn that filament number is the 7-0.9 dawn with method of the present invention, can be made into the finished fiber that filament number is the 2-0.2 dawn through hot drawing-off.The tensile strength of finished fiber is the 4-8 gram/dawn, and elongation at break is 15-70%.
The present invention intends briefly explaining advantage of the present invention and characteristics by some following embodiment and Comparative Examples.But should be noted that and to think that the present invention only limits to the content of embodiment.
Embodiment 1
Select the polypropylene resin composite (MI=26 of following prescription (seeing Table 1) for use, Q=2.0) melt spinning, spinning temperature need make resin fully melt evenly (being controlled at 260 ℃), is wound into silk for 400 meters/minute with wire winding speed, spin the filament number of undrawn yarn be respectively 3.6 dawn and 1.7 dawn.With hot drawing-off with they respectively drawing-off become the finished fiber that filament number is 1.1 dawn and 0.56 dawn.The tensile strength of finished fiber is respectively 5.3 gram/dawn and 5.7 gram/dawn, and elongation at break is 70% and 25%.And under identical (or similar) spinning, draw conditions, the polymer grade polypropylene resin made from the carrier model effective catalyst (is commonly referred to fiber-grade pp resin, MI=12.8 gram/the dawn, Q=1.43, Mw/ Mn ≈ 4-4.5) though can be wound into silk, but drawing-off smoothly can't be made the finished fiber of good mechanical properties.
The prescription of table 1 polypropylene resin composite
The carrier model efficient catalytic
Polymer grade polypropylene (MI=12.8, Q=1.43) 50 parts
Chemical degradation modified polypropene (MI=43, Q=1.27) 50 parts
0.1 part of calcium stearate
2,0.2 part of 6-di-tert-butyl-4-methy phenol (BHT)
1,010 0.2 parts of Irganox
(four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester)
HALS Tin 944(Ciba-Geigy) 0.2 part
Embodiment 2
Select for use the polypropylene resin composite of following three kinds of prescriptions (prescription sees Table 2-1) to carry out melt spinning, spinning temperature is 260 ℃, and wire winding speed is 400 meters/minute.These three kinds of acrylic resins all can successfully be spun into the undrawn yarn that filament number was about for 1.7 dawn, and all drawing-off successfully becomes the finished fiber at filament number＜0.6 dawn.The maximum drafting multiple of these undrawn yarns and the mechanical property of finished fiber are listed in table 2-2.
The prescription * of table 2-1 polypropylene resin composite
Numbering carrier model efficient catalytic polymer grade polypropylene chemical degradation modified polypropene
（MI＝12.8，Q＝1.43） （MI＝43，Q＝1.27）
90 parts 10 parts of 2-1
80 parts 20 parts of 2-2
70 parts 30 parts of 2-3
* other processing aids that added in this serial polypropylene resin composite are identical with the prescription of embodiment 1.
The character of table 2-2 polypropylene undrawn yarn and finished silk
The character of the finished fiber of polypropylene tree undrawn yarn
Fat numbering high draft multiple
Filament number tensile strength elongation at break
(dawn) (gram/dawn) (%)
2-1 4.5 0.54 5.9 50
2-2 4.5 0.60 5.9 30
2-3 4.4 0.55 5.2 20
Embodiment 3
Selecting the polypropylene resin composite of being made by the chemical degradation polypropylene of full-bodied polymer grade polypropylene (MI=1.4) and high fluidity for use is spinning PP Pipe Compound (prescription of these a series of polypropene compositions sees Table 3-1), carry out spinning at 230-260 ℃ spinning temperature respectively, be wound into silk with 400 meters/minute wire winding speeds.Spun undrawn yarn successfully drawing-off becomes fine denier filament, and the specification of the finished silk that makes is listed in table 3-2.The spinning contrast and experiment shows that the spinnability of polymer grade polypropylene resin obviously is lower than the selected polypropylene resin composite of the present invention.For example, be melt flow index that the spinning temperature of 1.4 polymer grade resin is elevated to 280 ℃ gradually by 230 ℃, all spinning smoothly; And aforesaid efficient catalytic polymer grade polypropylene resin (fibre resin) is though molecular weight distribution narrower (Q=1.43), can be wound into silk, but be difficult to drawing-off, its mechanical property do not reach far away the present invention with molecular weight distribution quite wide (Q=2.8) quality index of the fine count fiber that the polypropylene resin composite (seeing Table 3-1 and 3-2) of melt flow index similar with it (MI=12) is spun into.
The prescription * of table 3-1 polypropylene resin composite
Polypropylene polymer grade dimerization degradation modification polypropylene resin composite
Resin propylene component polypropylene component
Numbering (MI=1.4, Q=1.3) (MI=43, Q=1.27) MI Q
2 parts 98 parts 45 1.3 of 3-1
5 parts 95 parts 35 1.4 of 3-2
10 parts 90 parts 30 1.45 of 3-3
50 parts 50 parts 12 2.8 of 3-4
* other auxiliary agents that added in this serial polypropylene resin composite are identical with the prescription of embodiment 1.
The character of table 3-2 polypropylene undrawn yarn and finished silk
The character of polypropylene tree spinning warm rolling wrapping wire finished fiber
Fat numbering degree (℃) fiber number
(dawn) filament number tensile strength elongation at break
(dawn) (gram/dawn) (%)
3-1 235 2.4 0.67 5.4 15
3-2 255 1.7 0.43 7.8 21
3-3 235 2.5 - - -
3-4 260 2.4 0.82 5.6 75
3-4 260 1.7 0.53 5.7 80
Embodiment 4
Selecting the polymer grade polypropylene by the manufacturing of carrier model effective catalyst for use is raw material, handle the acrylic resin (MI=43 that makes high fluidity through the organic peroxide control degradation, Q=1.27, auxiliary agents such as the stabilizing agent of interpolation q.s, flow improving agent in this resin).The high-flowability polypropylene resin of this chemical modification is used for spinning, and spinning temperature is 235 ℃, and wire winding speed is 400 meters/minute, is spun into the undrawn yarn that filament number was 1.8 dawn, makes the fine count fiber that filament number was 0.53 dawn through overheated drawing-off again.The tensile strength of this finished silk was 8.0 gram/dawn, and extension at break is 25%.
Embodiment 5
Selecting 3-2 polypropylene resin composite used in the embodiment of the invention 3 for use is the spinning material, 230 ℃ of spinning, wire winding speed is respectively 500,600,800 and 1000 meters/minute, be wound into filament number and be respectively the undrawn yarn at 4.5,4.2,2.8 and 2.2 dawn, these thin dawn undrawn yarns all have good drawing-off performance, and its maximum drafting ratio is respectively 6.4,5.7,5.3 and 4.8 times.
Embodiment 6
In order to make the fine-denier polypropylene fiber of original liquid coloring, selecting 3-2 polypropylene resin composite used in the embodiment of the invention 3 for use is the spinning material resin.With per 100 parts of resins respectively with each 2 parts of mixing granulation of yellow masterbatch, red masterbatch and blue Masterbatch, make the polypropylene color section.These coloured sections can both be spun into the undrawn yarn that filament number is the 2.1-6.9 dawn with 245 ℃ spinning temperature and 400 meters/minute wire winding speed.But these undrawn yarns all have good drawdown.Its maximum drafting multiple is respectively 4.4-6.5 doubly (seeing table 4 for details)
Table 4
Acrylic resin undrawn yarn filament number maximum drafting multiple
(dawn)
Yellow acrylic resin 6.9 6.1
Composition 4.3 5.6
3.2 5.1
2.1 4.9
Red polypropylene resin 6.9 6.1
Composition 3.5 5.0
2.1 4.4
Blue look acrylic resin 6.9 6.5
Composition 2.1 4.7
Claims (5)
1, the manufacture method of thin dawn and superfine denier polypropylene fibers, it is characterized in that using the spinning PP Pipe Compound, the melt temperature of spinning PP Pipe Compound is 200-280 ℃ during spinning, wire winding speed be 300-1500 rice/minute, making filament number is the thin dawn undrawn yarn at 0.9-7 dawn, and thin dawn undrawn yarn is carried out hot drawing-off, and hot drawing temperature is 50-160 ℃, drafting multiple is 2.5-6 times, and making filament number is the thin dawn and the superfine denier polypropylene fibers at 0.2-2 dawn.
2, the manufacture method of thin dawn as claimed in claim 1 and superfine denier polypropylene fibers, the spinning PP Pipe Compound of using is the polypropylene resin composite that chemical degradation polypropylene, polymer grade polypropylene and processing aid (comprising stabilizing agent, flow improving agent, antistatic additive etc.) with high fluidity combine, its melt flow index is that 12-100(is preferably 30-50), polyacrylic molecular weight distributing index Q value is 1.3-4.0.
3, the manufacture method of thin dawn as claimed in claim 1 and superfine denier polypropylene fibers, the spinning PP Pipe Compound of using is the polypropylene resin composite made from chemical degradation of polypropylene resin and processing aid (comprising stabilizing agent, flow improving agent, antistatic additive etc.), its melt flow index is that 30-100(is preferably 30-50), polyacrylic molecular weight distributing index Q value is 1.1-1.5, used chemical degradation of polypropylene resin is to be raw material with the efficient catalytic polymer grade polypropylene resin, it is carried out chemical degradation and gets with a certain amount of organic peroxide.
4, the manufacture method of thin dawn as claimed in claim 1 and superfine denier polypropylene fibers, its thin dawn and superfine denier polypropylene fibers are to use as claim 2 or the described spinning PP Pipe Compound of claim 3, filament number is the 0.2-2 dawn, tensile strength is the 4-8 gram/dawn, elongation at break is 15-70%, the melt flow index of this polypropylene fibre is 12-100, and polyacrylic molecular weight distributing index Q value is 1.1-4.0.
5, the manufacture method of thin dawn as claimed in claim 1 and superfine denier polypropylene fibers, used spinning PP Pipe Compound is the polypropylene resin composite that is mixed with colouring agent, it is to form with the spinning PP Pipe Compound mixing granulation described in polypropylene Masterbatch and claim 2 or the claim 3, the filament number of making thin dawn and superfine denier polypropylene fibers is the 0.2-2 dawn, tensile strength is the 4-8 gram/dawn, and elongation at break is 15-70%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91104649 CN1027982C (en) | 1991-07-13 | 1991-07-13 | Preparing process of fine denier and ultra-fine denier polypropylene fibre P |
| GB929214837A GB9214837D0 (en) | 1991-07-13 | 1992-07-13 | Process for producing polyprophylene fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91104649 CN1027982C (en) | 1991-07-13 | 1991-07-13 | Preparing process of fine denier and ultra-fine denier polypropylene fibre P |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1068603A CN1068603A (en) | 1993-02-03 |
| CN1027982C true CN1027982C (en) | 1995-03-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91104649 Expired - Fee Related CN1027982C (en) | 1991-07-13 | 1991-07-13 | Preparing process of fine denier and ultra-fine denier polypropylene fibre P |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN1027982C (en) |
| GB (1) | GB9214837D0 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076032C (en) * | 1995-11-24 | 2001-12-12 | 中国科学院化学研究所 | Fine denier and super-fine denier polypropylene alloy fibre and its prodn. method |
| CN1068640C (en) * | 1997-09-24 | 2001-07-18 | 山东虎山实业集团有限公司 | Process for producing fine denier polypropylene fiber short-staple |
| CN1089380C (en) * | 1998-05-22 | 2002-08-21 | 孙世杰 | Fully drafting spinning process with high speed and low cost and its equipment |
| CN1123595C (en) * | 1998-08-31 | 2003-10-08 | 中国科学院化学研究所 | High-flowability polypropylene resin composition and its preparing process and usage |
| CN1068075C (en) * | 1998-08-31 | 2001-07-04 | 中国科学院化学研究所 | Low-temp spinning technique for polypropylene fibre |
| CN1116241C (en) * | 2000-04-26 | 2003-07-30 | 中国纺织大学化纤科技开发部 | Modified polypropene staple for concrete and mortar |
| TW579394B (en) * | 2001-04-24 | 2004-03-11 | Rhodia Industrial Yarns Ag | Process for the production of fine monofilaments made from polypropylene, fine monofilaments made from polypropylene, and their application |
| CN101058901B (en) * | 2006-04-07 | 2011-01-12 | 北京同道和诚科技发展有限公司 | Nano pearl polypropylene superfine Denier fibre and preparation method thereof |
| CN101812736B (en) * | 2010-03-16 | 2011-09-14 | 江苏丝丝缘纤维有限公司 | Production method of superfine polypropylene composite fully-drawn wallpaper fiber |
| CN102071488B (en) * | 2010-12-17 | 2012-05-30 | 北京中纺优丝特种纤维科技有限公司 | Sheath-core antibacterial colored polypropylene fiber and preparation method thereof |
| CN105200608B (en) * | 2015-06-29 | 2016-11-30 | 威尔克工业纺织（嘉兴）有限公司 | Waterproof and breathable uvioresistant polypropylene color-woven fabric |
| CN110872417B (en) * | 2018-08-29 | 2022-07-15 | 国家能源投资集团有限责任公司 | Spinning master batch, polypropylene fiber, preparation method of spinning master batch and polypropylene fiber, and polypropylene fiber product |
-
1991
- 1991-07-13 CN CN 91104649 patent/CN1027982C/en not_active Expired - Fee Related
-
1992
- 1992-07-13 GB GB929214837A patent/GB9214837D0/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| CN1068603A (en) | 1993-02-03 |
| GB9214837D0 (en) | 1992-08-26 |
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