CN104695083B - A kind of heat stretching process of aramid III fiber raw tow - Google Patents
A kind of heat stretching process of aramid III fiber raw tow Download PDFInfo
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- CN104695083B CN104695083B CN201510131346.XA CN201510131346A CN104695083B CN 104695083 B CN104695083 B CN 104695083B CN 201510131346 A CN201510131346 A CN 201510131346A CN 104695083 B CN104695083 B CN 104695083B
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/224—Selection or control of the temperature during stretching
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
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- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
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Abstract
The heat stretching process of a kind of aramid III fiber raw tow disclosed by the invention, it is characterised in that the heat stretching process is divided into the progress of two steps：The first step be by the raw tow of aramid III fiber in 270~300 DEG C low temperature, identical tension be 0.2 1.0cN/tex under carry out hot-stretch; second step is that the fiber after the first step is handled continues to stretch under 0.01~0.2cN/tex of identical tension in 340 500 DEG C, and two sections of hot-stretch are carried out under normal pressure inert gas shielding.Because the present invention uses two step heat stretching process, and the first step therein is progress identical tension hot-stretch at low temperature, the glass transition temperature for not only taking full advantage of fiber at this temperature is relatively low, the characteristics of stretching for being more beneficial for macromolecular chain is orientated, in addition the tension force for designing application is larger, the degree of orientation of aramid III finished fiber is thus substantially increased, its tensile strength and initial modulus is all improved.Present invention process is simple to operate, and cost is relatively low, and technical maturity is conducive to industrialized production.
Description
Technical field
The invention belongs to chemical fibre spinning tow heat stretching process technical field, and in particular to a kind of high intensity, Gao Mo
The heat stretching process of the aramid III fiber raw tow of amount.
Background technology
With the development of space technology, higher and higher requirement is proposed with fiber to enhancing.Past, in the world to aramid fiber
Research be that but the tensile strength of the serial fiber can only achieve 22cN/dt or so for main object with U.S. kevlar series,
This can not meet requirements at the higher level of the aerospace field to the mechanical property of advanced composite material enhancing fiber.Aramid III
Fiber (Russia is called Armos fibers) has turned into prepare aviation boat at present as a kind of high strength and modulus organic fiber
The reinforcing fiber of its advanced composite material.In this regard, Russ P RU2074182 and RU2130980 describe this resin and
The production technology of fiber, it is specifically by p-phenylenediamine, paraphthaloyl chloride and 5 (6)-amido -2- (4- aminocarbonyl phenyls) benzo
Three kinds of monomers of imidazoles are raw material, obtain spinning solution through low temperature copolymerization by solvent of dimethyl acetamide/lithium chloride, then pass through
The techniques such as filter, deaeration, spinning, washing, drying and winding obtain aramid III precursor, and the general tensile strength of the raw tow only has 8
~10cN/dt, it is necessary to which finished fiber beam can just be obtained by being heat-treated to raw tow.Such as to the heat treatment side of the fiber precursor beam
Method, RU2167961 reports a kind of batch (-type) heat treatment method, and this method is the silk cylinder that will be wound into spinning process, is put into
In the heat treatment kettle of multistation, after nitrogen displacement, kept for more than 30 minutes under vacuum condition, being warming up to 300-400 DEG C, then
Cool nitrogen charging, and it is finished fiber to drive kettle and take out silk cylinder.But finished fiber tensile strength (the dry yarn, non-leaching that this method is obtained
Collodion silk) in more than 26cN/dt qualification rate it is only 70-80%.The problem of existing for RU2167961, CN 1473969A are disclosed
A kind of step heat stretching process, the technique is in constant-tension (0.2-1.0cN/tex) nitrogen by aramid III fiber raw tow
Under protection, online hot-stretch is carried out in 340-500 DEG C of heater, although improve to a certain extent aramid III into
The yield rate of product fiber, when overcoming in interval Technology for Heating Processing silk cylinder and being heated in heating kettle, the inside and outside layer tow existed by
Tow is heated uneven and causes the problem of product qualification rate is low between cylinder and cylinder on hot uneven and multistation, but not ideal enough.Therefore,
The mechanical property for how further improving aramid III fiber is still current scientific worker's technical issues that need to address.
The content of the invention
The purpose of the present invention is the drawbacks described above existed for the existing step heat stretching process of aramid III fiber precursor one, is carried
For a kind of new technique that hot-stretch is carried out to aramid III fiber raw tow, the technique can obtain aramid III fiber finished silk
High intensity and high-modulus, and process is simple, operation is easy.
In order to reach the purpose of the present invention, the present inventor enters to the existing step heat stretching process of aramid III fiber precursor one
Deep analysis and research is gone, has found to be complexed material on benzimidazole structure contained in aramid III raw tow macromolecular chain
Expect accessory substance HCl (see Fig. 1) in polycondensation process, the HCl of the complexing destroy in polymer macromolecule chain benzimidazole it
Between interaction of hydrogen bond (as shown in Figure 2), the interaction force of macromolecular chain is reduced, so as to significantly reduce raw tow
Glass transition temperature, makes 276 DEG C before being complexed of its glass transition temperature be reduced to 254 DEG C (see Fig. 3).Study simultaneously
In it has also been found that the temperature of the HCl solution complexings (abjection) of aramid III fiber precursor complexing is 300~330 DEG C (see Fig. 3).Although existing
The step heat stretching process having can make the HCl being complexed in precursor solve complexing, but because it is the online hot-drawn of a step at high temperature
Stretch, because being complexed HCl rapid solution complexing, the interaction of intermolecular hydrogen bonding is increased, so as to be unfavorable for the tensility of precursor
Raising, cause the increase of its intensity and modulus limited.
On the basis of analysing in depth and study more than, the present invention provides following such a technical solution to reach
Goal of the invention：
The raw tow of aramid III fiber is subjected to two step hot-stretch；The first step be by the raw tow of aramid III fiber in
Identical tension hot-stretch is carried out in a low temperature of 270~300 DEG C, second step is the fiber for handling the first step in 340-500 DEG C of continuation
Stretched under identical tension, two sections of hot-stretch are carried out under normal pressure inert gas shielding.
Preferably 280~290 DEG C of the temperature of first step identical tension hot-stretch described in process above；Second step identical tension heat
Preferably 380~420 DEG C of the temperature of stretching.
The tension force of first step identical tension hot-stretch described in process above is 0.2-1.0cN/tex, preferably 0.5-
0.8cN/tex, processing time is 1-5 minutes, preferably 2-3 minutes.
The tension force of second step identical tension hot-stretch described in process above is 0.01~0.2cN/tex, preferably 0.05-
0.1cN/tex, processing time is 0.5-5 minutes, preferably 1-2 minutes.
Inert gas described in process above is any of nitrogen, argon gas, helium or carbon dioxide.
The degree of orientation with the aramid III finished fiber of gained after above PROCESS FOR TREATMENT is 0.89-0.92, tensile strength 29-
33cN/dt, initial modulus is 980-1050cN/dt.
The present invention compared with prior art, has the positive effect that：
1st, because the present invention uses two step heat stretching process, and the first step therein is to carry out permanent at low temperature
Power hot-stretch, not only takes full advantage of the HCl that benzimidazole unit is complexed in macromolecular chain at this temperature and not yet removes, complexing
HCl destroys the interaction of hydrogen bond between benzimidazole unit in macromolecular chain, and the glass transition temperature of fiber is relatively low, more has
The characteristics of being orientated beneficial to the stretching of macromolecular chain, the tension force that application is designed in addition is larger, thus substantially increases aramid III finished product
The degree of orientation of fiber, makes its tensile strength and initial modulus all be improved, and overcomes the published steps of CN 1473969A
In method hot-stretching step, aramid III fiber raw tow is placed in moment under 340-500 DEG C of hot environment, and the HCl of complexing is solved rapidly
The problem of tensility for being unfavorable for precursor produced by being complexed and increasing intermolecular interaction is improved.
2nd, because the present invention uses two step heat stretching process, and the first step therein is to carry out permanent at low temperature
Power hot-stretch, thus the stretching orientation of macromolecular chain is not only contributed to, and also help the solvent remained in raw tow and can delay
It is slow to be escaped from fibrous inside so that fibrous inside hole is reduced, and one-step method hot-drawn disclosed in CN 1473969A can be reduced or avoided
During stretching, a small amount of solvent is remained in aramid III fiber raw tow in 340 DEG C of high temperature and its above abrupt release, can be caused
The problem of there is hole inside aramid III fiber.
3rd, because the heat stretching process that the present invention is provided will not change existing equipment device etc., thus simple to operate, cost
Relatively low, technical maturity is conducive to industrialized production.
Brief description of the drawings：
Fig. 1 is the INFRARED SPECTRUM for not being complexed HCl aramid IIIs (curve a, dotted line) and complexing HCl aramid IIIs (curve b, solid line)
Figure.Wherein curve b is shown in 2500~2900cm-1Have and substantially belong to N+- H vibration peaks, illustrate HCl complexings in aramid III
On macromolecular chain；While 3400~3500cm-1The N-H vibrations for not forming hydrogen bond are belonged to, clearly it can be seen that network from figure
Closing HCl aramid IIIs, (appearance becomes apparent from curve b) in this place, illustrates that the hydrogen bond not formed is more, interaction of hydrogen bond is weak.
Fig. 2 is the structure after the structure and solution complexing HCl of benzimidazole unit in complexing HCl aramid III macromolecular chains
Schematic diagram.
Fig. 3 is loss tangent (Tan Delta)/temperature obtained by aramid III fiber dynamic mechanical analysis (DMA) are tested
Degree figure, the wherein corresponding temperature of peak of curve are glass transition temperature.Solution is complexed HCl aramid III fibers as seen from the figure
Glass transition temperature is 276 DEG C (a curves), and the glass transition temperature for being complexed HCl aramid III fiber is 254 DEG C of (b
Curve).
Fig. 4 is heat analysis (TGA) test chart of aramid III fiber raw tow under 10 DEG C/min of heating rate.T1 in figure
=300 DEG C are HCl starting abjection temperature, and T2=330 DEG C is the completely out temperature of HCl.
Fig. 5 be the embodiment of the present invention 1 in after two step hot-stretch aramid III fiber finished silk Two dimensional X ray diffraction
(XRD) test chart.
Fig. 6 tests for the Two dimensional X ray diffraction (XRD) of aramid III fiber finished silk after a step hot-stretch in comparative example 1
Figure.
Comparison diagram 5,6, can clearly see that diffraction speck is brighter in Fig. 5, it is narrower to be distributed, illustrate that its degree of orientation is higher.
Embodiment
Embodiment is given below so that the invention will be further described.It is necessarily pointed out that following examples can not
Be interpreted as limiting the scope of the invention, if the person skilled in the art in the field according to the invention described above content to this hair
It is bright to make some nonessential modifications and adaptations, still fall within the scope of the present invention.
In addition, what deserves to be explained is, 1) degree of orientation of following examples and the aramid III finished fiber obtained by comparative example is
Using Two dimensional X ray diffraction instrument --- De Luke (Bruker D8) diffractometer is tested, and according to following fiber-wall-element model degree meter
Calculate formula and calculate what is obtained：
Wherein φ is azimuth, and I (φ) is the scanning intensity of azimuth φ, f2It is referred to as Herman orientation factors, is used for
Fiber-wall-element model degree is represented, the degree of orientation is bigger, illustrates that fiber is better along draw direction degree of orientation.2) following examples and contrast
The tensile strength and initial modulus of aramid III finished fiber obtained by example are to use Britain Instron4302 type strength testers, according to
ASTM D885-2007 method, according to fixture spacing 215mm, fixture translational speed 25mm/min, simple tension test.
Embodiment 1
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 600cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 0.6cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature
To handle 3min in 285 DEG C of first paragraph heating furnace, then tensile stress is adjusted and protected to 0.08cN/tex into normal pressure nitrogen
Under shield, furnace temperature is handles 2min in 400 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.92, and tensile strength is 33cN/dt, and initial modulus is 1010cN/dt.
Embodiment 2
It is the raw tow that 8cN/dt, modulus are the aramid III fiber that 500cN/dt, fiber number are 95tex by intensity, being placed in can
On the transfer roller rotated freely, tension force is stretched to through tensioner after 0.5cN/tex, to be placed under the protection of normal pressure argon gas, furnace temperature is
5min is handled in 270 DEG C of first paragraph heating furnace, then tensile stress is adjusted and protected to 0.01cN/tex into normal pressure argon gas
Under, furnace temperature is handles 0.5min in 500 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.90, and tensile strength is 30cN/dt, and initial modulus is 980cN/dt.
Embodiment 3
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 600cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 1cN/tex, to be placed under the protection of normal pressure helium, furnace temperature is
1min is handled in 290 DEG C of first paragraph heating furnace, then tensile stress is adjusted and protected to 0.2cN/tex into normal pressure helium
Under, furnace temperature is handles 5min in 450 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.91, and tensile strength is 30cN/dt, and initial modulus is 1050cN/dt.
Embodiment 4
It is the raw tow that 9cN/dt, modulus are the aramid III fiber that 550cN/dt, fiber number are 95tex by intensity, being placed in can
On the transfer roller rotated freely, tension force is stretched to through tensioner after 0.8cN/tex, to be placed on normal pressure CO 2 gas-shielded
Under, then tensile stress is adjusted to 0.1cN/tex to handle 4min in 280 DEG C of first paragraph heating furnace and enters normal pressure by furnace temperature
Under CO 2 gas-shielded, furnace temperature is handles 1min in 340 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished product
Fiber.
The degree of orientation of the fiber is 0.88, and tensile strength is 29cN/dt, and initial modulus is 980cN/dt.
Embodiment 5
It is the raw tow that 9cN/dt, modulus are the aramid III fiber that 550cN/dt, fiber number are 95tex by intensity, being placed in can
On the transfer roller rotated freely, tension force is stretched to through tensioner after 0.2cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature is
2.5min is handled in 300 DEG C of first paragraph heating furnace, then tensile stress is adjusted and protected to 0.05cN/tex into normal pressure nitrogen
Under shield, furnace temperature is handles 1.5min in 420 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.91, and tensile strength is 31cN/dt, and initial modulus is 1010cN/dt.
Embodiment 6
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 580cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 0.4cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature
To handle 2min in 275 DEG C of first paragraph heating furnace, then tensile stress is adjusted and protected to 0.04cN/tex into normal pressure nitrogen
Under shield, furnace temperature is handles 4min in 380 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.91, and tensile strength is 30cN/dt, and initial modulus is 1020cN/dt.
Embodiment 7
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 560cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 0.9cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature
To handle 1.8min in 295 DEG C of first paragraph heating furnace, then tensile stress is adjusted to 0.14cN/tex and enters normal pressure nitrogen
Under protection, furnace temperature is handles 0.8min in 360 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.91, and tensile strength is 31cN/dt, and initial modulus is 1010cN/dt.
Embodiment 8
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 600cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 0.7cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature
To handle 3.5min in 285 DEG C of first paragraph heating furnace, then tensile stress is adjusted to 0.05cN/tex and enters normal pressure nitrogen
Under protection, furnace temperature is handles 1min in 420 DEG C of the hot stove of second segment, and finally winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.92, and tensile strength is 32cN/dt, and initial modulus is 1050cN/dt.
Comparative example 1
It is the raw tow that 10cN/dt, modulus are the aramid III fiber that 600cN/dt, fiber number are 95tex by intensity, is placed in
On rotatable transfer roller, tension force is stretched to through tensioner after 0.6cN/tex, to be placed under nitrogen protection under normal pressure, furnace temperature
To handle 5min in 400 DEG C of heating furnaces, then winding turns into aramid III finished fiber.
The degree of orientation of the fiber is 0.86, and tensile strength is 28cN/dt, and initial modulus is 900cN/dt.
Claims (7)
1. a kind of heat stretching process of aramid III fiber raw tow, it is characterised in that the heat stretching process is divided into the progress of two steps：
The first step is that the raw tow of aramid III fiber is carried out into identical tension hot-stretch, second step in a low temperature of 270~300 DEG C
It is that the fiber after the first step is handled continues to stretch under identical tension in 340-500 DEG C, two sections of hot-stretch are in normal pressure indifferent gas
Body protection is lower to be carried out.
2. the heat stretching process of aramid III fiber raw tow according to claim 1, it is characterised in that described in the technique
First step identical tension hot-stretch temperature be 280~290 DEG C.
3. the heat stretching process of aramid III fiber raw tow according to claim 1 or 2, it is characterised in that in the technique
The temperature of described second step identical tension hot-stretch is 380~420 DEG C.
4. the heat stretching process of aramid III fiber raw tow according to claim 1 or 2, it is characterised in that in the technique
The tension force of described first step identical tension hot-stretch is 0.2-1.0cN/tex, and processing time is 1-5 minutes；Second step identical tension
The tension force of hot-stretch is 0.01~0.2cN/tex, and processing time is 0.5-5 minutes.
5. the heat stretching process of aramid III fiber raw tow according to claim 3, it is characterised in that described in the technique
First step identical tension hot-stretch tension force be 0.2-1.0cN/tex, processing time be 1-5 minutes；Second step identical tension hot-drawn
The tension force stretched is 0.01~0.2cN/tex, and processing time is 0.5-5 minutes.
6. the heat stretching process of aramid III fiber raw tow according to claim 1 or 2, it is characterised in that in the technique
The tension force of described first step identical tension hot-stretch is 0.5-0.8cN/tex, and processing time is 2-3 minutes；Second step identical tension
The tension force of hot-stretch is 0.05-0.1cN/tex, and processing time is 1-2 minutes.
7. the heat stretching process of aramid III fiber raw tow according to claim 3, it is characterised in that described in the technique
First step identical tension hot-stretch tension force be 0.5-0.8cN/tex, processing time be 2-3 minutes；Second step identical tension hot-drawn
The tension force stretched is 0.05-0.1cN/tex, and processing time is 1-2 minutes.
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| CN106758136B (en) * | 2016-12-29 | 2019-04-05 | 四川大学 | Aromatic polymer fiber and preparation method thereof of the high composite performance containing benzimidazole |
| CN109797542A (en) * | 2017-11-17 | 2019-05-24 | 中蓝晨光化工有限公司 | A kind of preparation method of plating metal on surface aramid fiber |
| CN112301443B (en) * | 2019-08-01 | 2022-04-12 | 中蓝晨光化工有限公司 | Three-stage heat setting method of heterocyclic aramid fiber |
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| RU2017866C1 (en) * | 1992-08-04 | 1994-08-15 | Черных Татьяна Егоровна | Molded article |
| CN1293240C (en) * | 2002-08-06 | 2007-01-03 | 中蓝晨光化工研究院 | Post-treatment new process for aramid fibre III raw tow |
| KR101403301B1 (en) * | 2006-11-21 | 2014-06-05 | 데이진 아라미드 비.브이. | Method for obtaining high-tenacity aramid yarn |
| CN101787582B (en) * | 2010-02-10 | 2011-09-28 | 中蓝晨光化工研究院有限公司 | Preparation method of high-tensile high-model heterocycle aramid fiber |
| CN101798720B (en) * | 2010-04-28 | 2011-07-27 | 四川辉腾科技有限公司 | Aramid fiber III on-line thermal treating process and device thereof |
| JP5960167B2 (en) * | 2011-01-13 | 2016-08-02 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーＥ．Ｉ．Ｄｕ Ｐｏｎｔ Ｄｅ Ｎｅｍｏｕｒｓ Ａｎｄ Ｃｏｍｐａｎｙ | Copolymer fiber and yarn and method for producing copolymer fiber and yarn |
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| 含杂环的芳香族共聚酰胺纤维在热处理过程中的结构与性能研究;唐国平;《中国优秀硕士学位论文全文数据库》;20130630;第9-30页 * |
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