CN102560700A - Para-aramid fine denier fiber and preparation method thereof - Google Patents
Para-aramid fine denier fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to para-aramid fine denier fiber and a preparation method thereof. The method comprises the following steps: dissolving a para-aramid polymer in a strong acid, filtering twice, defoaming, performing tertiary filtration, spinning, stretching, cooling to solidify, rinsing, drying and rolling to finally prepare the finished fiber. In the preparation method, a high shear double screw extruder and a continuous film defoaming device are adopted, multiple filtering working procedures are adopted, the filtering precision characterized by the filtering plugging value Kw which is no more than 150, the defoaming purity, the spinning temperature, the stretching condition and the like are strictly controlled, the global optimization of process steps and process conditions is performed, the method is practical and is high in operability, and the para-aramid fine denier fiber with good physical properties can be prepared. The para-aramid fine denier fiber has the advantages of high strength and good quality, the fineness is 30-100D, the tensile strength is no less than 22CN/dtex, the elongation at break is no less than 2.5% and the initial modulus is no less than 550CN/dtex.
Description
Technical field
The invention belongs to field of textiles, be specifically related to a kind of p-aramid fiber fine count fiber and preparation method thereof
Background technology
aramid fiber is a kind of high-tech special fibre, has broad application prospects in fields such as high strength tire and rubber industry, bullet resistant material and protective clothes, friction sealed insulating materials, space flight and aviation structural member, the wear-resistant composite of high-strength impact-resistant, the heat-resisting cables of high-strength corrosion-resisting.Progress along with aramid fiber preparation technology; The progressively expansion of producing; And aramid fiber good insulation performance property and corrosion resistance; Make it also enlarge rapidly in the application of aspects such as fiber reinforcement cable, communication electronic equipment, especially communication electronic equipment aspect increases the increasing demand of aramid fiber fine count fiber.
In
prior art; Preparation para-aramid fiber (being Fanglun l414) topmost process is: adopting paraphthaloyl chloride and p-phenylenediamine (PPD), is that dicyandiamide solution carries out the cryogenic fluid polycondensation and obtains the p-aramid fiber condensate with N-Methyl pyrrolidone/calcium chloride; This p-aramid fiber condensate obtains para-aramid fiber through washing, filtration, sulfuric acid dissolution, filtration, deaeration, spinning, washing, drying and rolling again.This production method exists the following deficiency: when 1) the p-aramid fiber condensate is dissolved in the strong acid system such as the concentrated sulfuric acid dissolving inhomogeneous, have gel particles, these gel particles can influence spinning effect, even make normally spinning; 2) the aramid fiber condensate in the concentrated sulfuric acid with dissolution time increase, aggravation is degraded in the raising of solution temperature, this is easy to influence the physical property of finished fiber; 3) because the high deaeration of solution viscosity difficulty, residue gas is steeped oneself-meeting and is caused lousiness and broken end, even make can't ordinary production, and this influence for fine count fiber is particularly evident
Summary of the invention
technical problem to be solved by this invention is the deficiency that overcomes prior art, and a kind of preparation method of improved p-aramid fiber fine count fiber is provided.
For solving above technical problem, the present invention takes following technical scheme:
A kind of preparation method of p-aramid fiber fine count fiber comprises the steps:
(1), strong acid is mixed with the p-aramid fiber condensate mutually, the gained compound is sent in the high shear double screw extruder again and is dissolved, dissolution time obtained the p-aramid fiber polymer solution between 15 ~ 30 minutes;
(2), making step (1) gained solution first is that 500 ~ 800 purpose filters carry out the filtration first time through the filter screen precision, is that 1000 ~ 1500 purpose filters carry out the filtration second time through the filter screen precision again;
(3), the filtrating that step (2) filtration is for the second time obtained is sent into the continuous film defoaming device and is carried out deaeration;
(4), will passing through after step (3) deaeration solution of gained, to send into the filter screen precision again be that 1500 ~ 2500 purpose filters filter for the third time;
(5), will pass through the filtrating that obtains after step (4) is filtered for the third time and send into filament spinning component and spray silk, stretch, send into the cooled and solidified groove again and carry out cooled and solidified, form fiber; When silk control spray, the spinneret cap temperature was between 88 ~ 95 ℃, during stretching the air layer height between 5 ~ 16 millimeters, draw ratio is 4.5 ~ 8 times;
The gained fiber makes described p-aramid fiber fine count fiber finished product again through alkali cleaning, washing, drying and rolling after
(6), step (5) cooled and solidified.
preferably, in the step (1), the mass fraction that said p-aramid fiber condensate accounts for the p-aramid fiber polymer solution is 18 ~ 21%.
are as optimal way of the present invention; The double screw extruder that employed high shear double screw extruder is following structure in the step (1): the first half of two intermeshing twin-screws is to be combined by the kneading piece of various forward thread bush, different rotation directions and a spot of reverse thread cover; The total length of wherein mediating piece accounts for more than 30% of this partial-length; More preferably, the latter half of twin-screw is made up of the thread bush that reduces gradually along Way out pitch.Specifically can select the patent No. is employed double screw extruder in the patent of ZL 200510030946.3.Among the present invention; For preventing that the p-aramid fiber condensate from aggravating with the degraded that dissolution time increases, solution temperature improves in strong acid; Adopt high shear double screw extruder and strict control dissolution time, make the p-aramid fiber condensate can realize quick dissolving, finally improve the intensity of fibre.
are as another optimal way of the present invention; The structure of said continuous film defoaming device is following: by the charging basket of jacketed, be arranged in the charging basket and and the charging basket inwall between leave the gap sector, be used to drive the transmission device of sector rotation, and the charging aperture that points to sector constitutes; And sector can form funnel with the charging basket inwall on 360 ° of directions in rotary course, makes the material that gets in the said charging basket from said charging aperture under the rotary centrifugal force effect, forming film on the sector.Specifically can select the patent No. is the manufacturing homogeneity Fanglun 1414's described in the patent of ZL 200720066149.5 continuous defoaming device.The present invention uses this continuous film defoaming device that the effusion stroke of bubble in the spinning solution is shortened greatly, rapidly defoaming under the effect of realization condition of high vacuum degree, and the degree of purity after the spinning solution deaeration is also higher simultaneously.
in addition, 5 ~ 10 times of injection diameter preferably of the distance between the spray orifice on the spinneret cap in the step (5).
are in the preparation process of p-aramid fiber fine count fiber; Because fibre diameter is thin, the spinneret orifice number is few; So the uniformity and the degree of purity of slurry are very big to the influence of goods before the spinning; The present invention adopts at least three roads to filter operation before spinning, has improved the uniformity and the degree of purity of p-aramid fiber polymer solution, has guaranteed the quality of fibrous finished product.
because the viscosity of p-aramid fiber polymer solution is high, deaeration is difficult, residue gas is steeped oneself-meeting and is caused lousiness, broken end.The every intrafascicular hole count of general fibre (being radical) is hundreds of nearly, a small amount of lousiness occurs, the broken end influence is little, but for the every intrafascicular hole count of fine count fiber seldom, and minimum have only 20 holes, so in case a lousiness appears, broken end will cause can't ordinary production.Therefore, the deaeration process also is vital for the production of fine count fiber, and the present invention adopts the continuous film defoaming device that solution is carried out deaeration, can realize rapidly defoaming; Select certain high temperature for use during the spray silk, suitably reduce solution viscosity, can prevent to extrude fracture of wire because of the drop type; In addition, the control stretching process conditions, specific area increased when fiber was pulled out, and cooled and solidified is even, and every fiber all evenly spins well in the time of can guaranteeing spinning; Significantly reduce lousiness and broken end phenomenon in the spinning process.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
preparation method of the present invention is through adopting special-purpose high shear double screw extruder and special-purpose continuous film defoaming device; Filter operation through multiple tracks, the spray silk temperature in the strict control spinning process, stretching condition etc. have carried out the global optimization of processing step and process conditions; Implement easily; Workable, concrete advantage has: 1) deaeration efficient is high, and deaeration is thoroughly complete; 2) the spinning solution filterability is good, and high purity filters plugging value Kw≤150; 3) lousiness in the spinning process and broken end phenomenon have effectively been avoided.
The p-aramid fiber fine count fiber intensity that
the present invention makes is high, quality is good, has good physical property; The fibre number scope between 30 ~ 100 dawn, TENSILE STRENGTH>=22CN/dtex, elongation at break>=2.5%, initial modulus>=550CN/dtex.
The specific embodiment
are done further detailed explanation below in conjunction with concrete embodiment to the present invention, but are not limited to these embodiment.
Embodiment 1
The preparation method of the p-aramid fiber fine count fiber of present embodiment, detailed process is following:
(1), in the 10L kneading machine, to add the 6L mass concentration be 99.98% the concentrated sulfuric acid; Stir down toward wherein adding the p-aramid fiber condensate; Both are mixed mutually, then compound is sent into dissolving 20min in the special-purpose high shear double screw extruder (patent No.: ZL 200510030946.3), obtain the p-aramid fiber polymer solution; In this example, the polymeric mass fraction of p-aramid fiber accounts for 18.5% of this solution.
(2), p-aramid fiber polymer solution that step (1) is obtained is pressed into filter screen 800 purpose filters 1 and carries out the first time and filter, and then carries out filtration second time through screen pack 1500 purpose filters 2;
(3), will pass through filtrating that step (2) twice filtration obtain sends into special-purpose continuous film defoaming device (patent No.: ZL 200720066149.5) and removes bubble;
(4), will passing through after step (3) deaeration solution of gained, to send into the filter screen precision again be that 2500 purpose filters 3 filter for the third time, and K is surveyed in sampling
W
Value is 110;
(5), will pass through the filtrating that obtains after step (4) is filtered for the third time and send into filament spinning component, filtrating is extruded from spinneret cap through metering, the spinneret orifice spacing is 0.8 millimeter, the spinneret cap temperature is controlled at 88 ℃; The silk of ejection stretches through the air-gap of a height at 10 millimeters, and draw ratio is about 8 times; Get into the cooled and solidified groove then, carry out cooled and solidified, form fiber;
The gained fiber is again through alkali cleaning, washing, drying and rolling after
(6), step (5) cooled and solidified, and making fiber number is the p-aramid fiber fine count fiber finished product at 30 dawn.Record the TENSILE STRENGTH of this fiber: >=23CN/dtex; Elongation at break: >=2.5%; Initial modulus: >=600 CN/dtex.
are because the non-constant of p-aramid fiber condensate dissolubility; So can only be dissolved in the strong acid systems such as the concentrated sulfuric acid; And dissolve whether evenly extremely importantly to spinning; If dissolving is inhomogeneous thorough, then have gel particles, these gel particles can have a strong impact on the quality of spinning and fiber product too much.Adopt viscose spinning examination criteria method to survey the filtration plugging value (Kw value) of p-aramid fiber polymer solution among the present invention, characterize the strainability of p-aramid fiber polymer solution with the Kw value.
The computing formula of Kw value is following:
Kw＝10
5
×[（2－P
2
／P
1
）／(P
1
＋P
2
)]
In
formula: the solution amount through filter medium behind the 20min under the P1=constant voltage.
Pass through the solution amount of regulation filter medium in
same test of P2=behind the continuation mensuration 40min.
Kw value is more little, shows that then the strainability of solution is good more, gel particles is few more.
In the present embodiment, through the K of the polymer solution after filtering for the third time
W
Value is 110, and the K of general similar fine count fiber when preparing
W
All about 200, the spinning slurry of this explanation present embodiment has good filterability to value, and is very favourable for spinning.
Embodiment 2
The preparation method of the p-aramid fiber fine count fiber of present embodiment, detailed process is following:
(1), in the 10L kneading machine, to add the 5L mass concentration be 99.98% the concentrated sulfuric acid; Stir down toward wherein adding the p-aramid fiber condensate; Both are mixed mutually, then compound is sent into dissolving 25min in the special-purpose high shear double screw extruder (patent No.: ZL 200510030946.3), obtain the p-aramid fiber polymer solution; In this example, the polymeric mass fraction of p-aramid fiber accounts for 19.5% of this solution.
(2), p-aramid fiber polymer solution that step (1) is obtained is pressed into filter screen 600 purpose filters 1 and carries out the first time and filter, and then carries out filtration second time through screen pack 1200 purpose filters 2;
(3), will pass through the filtrating that step (2) twice filtration obtain and send into the special-purpose continuous film defoaming device (patent No.: 200720066149.5) remove bubble;
(4), will passing through after step (3) deaeration solution of gained, to send into the filter screen precision again be that 2500 purpose filters 3 filter for the third time, and K is surveyed in sampling
W
Value is 120;
(5), will pass through the filtrating that obtains after step (4) is filtered for the third time and send into filament spinning component, filtrating is extruded from spinneret cap through metering, the spinneret orifice spacing is 0.6 millimeter, the spinneret cap temperature is controlled at 89 ℃; The silk of ejection stretches through the air-gap of a height at 14 millimeters, and draw ratio is about 6 times; Get into the cooled and solidified groove then, carry out cooled and solidified, form fiber;
The gained fiber is again through alkali cleaning, washing, drying and rolling after
(6), step (5) cooled and solidified, and making fiber number is the p-aramid fiber fine count fiber finished product at 50 dawn.Record the TENSILE STRENGTH of this fiber: >=23CN/dtex; Elongation at break: >=2.5%; Initial modulus: >=550CN/dtex.
Embodiment 3
The preparation method of the p-aramid fiber fine count fiber of present embodiment, detailed process is following:
(1), in the 10L kneading machine, to add the 5L mass concentration be 99.98% the concentrated sulfuric acid; Stir down toward wherein adding the p-aramid fiber condensate; Both are mixed mutually, then compound is sent into dissolving 30min in the special-purpose high shear double screw extruder (patent No.: ZL 200510030946.3), obtain the p-aramid fiber polymer solution; In this example, the polymeric mass fraction of p-aramid fiber accounts for 20% of this solution.
(2), p-aramid fiber polymer solution that step (1) is obtained is pressed into filter screen 700 purpose filters 1 and carries out the first time and filter, and then carries out filtration second time through screen pack 1500 purpose filters 2;
(3), will pass through the filtrating that step (2) twice filtration obtain and send into the special-purpose continuous film defoaming device (patent No.: 200720066149.5) remove bubble;
(4), will passing through after step (3) deaeration solution of gained, to send into the filter screen precision again be that 2500 purpose filters 3 filter for the third time, and K is surveyed in sampling
W
Value is 110;
(5), will pass through the filtrating that obtains after step (4) is filtered for the third time and send into filament spinning component, filtrating is extruded from spinneret cap through metering, the spinneret orifice spacing is 0.4 millimeter, the spinneret cap temperature is controlled at 88 ℃; The silk of ejection stretches through the air-gap of a height at 10 millimeters, and draw ratio is about 8 times; Get into the cooled and solidified groove then, carry out cooled and solidified, form fiber;
The gained fiber is again through alkali cleaning, washing, drying and rolling after
(6), step (5) cooled and solidified, and making fiber number is the p-aramid fiber fine count fiber finished product at 100 dawn.Record the TENSILE STRENGTH of this fiber: >=22CN/dtex; Elongation at break: >=2.5%; Initial modulus: >=550 CN/dtex.
More than the present invention has been done detailed description; Its purpose is to let the personage that is familiar with this art can understand content of the present invention and implements; Can not limit protection scope of the present invention with this; All equivalences of doing according to spirit of the present invention change or modify, and all should be encompassed in protection scope of the present invention
Claims (8)
1. the preparation method of a p-aramid fiber fine count fiber is characterized in that: comprise the steps:
(1), strong acid is mixed with the p-aramid fiber condensate mutually, the gained compound is sent in the high shear double screw extruder again and is dissolved, dissolution time obtained the p-aramid fiber polymer solution between 15 ~ 30 minutes;
(2), making step (1) gained solution first is that 500 ~ 800 purpose filters carry out the filtration first time through the filter screen precision, is that 1000 ~ 1500 purpose filters carry out the filtration second time through the filter screen precision again;
(3), the filtrating that step (2) filtration is for the second time obtained is sent into the continuous film defoaming device and is carried out deaeration;
(4), will passing through after step (3) deaeration solution of gained, to send into the filter screen precision again be that 1500 ~ 2500 purpose filters filter for the third time;
(5), will pass through the filtrating that obtains after step (4) is filtered for the third time and send into filament spinning component and spray silk, stretch, send into the cooled and solidified groove again and carry out cooled and solidified, form fiber; When silk control spray, the spinneret cap temperature was between 88 ~ 95 ℃, during stretching the air layer height between 5 ~ 16 millimeters, draw ratio is 4.5 ~ 8 times;
(6), the gained fiber makes described p-aramid fiber fine count fiber finished product again through alkali cleaning, washing, drying and rolling after step (5) cooled and solidified.
2. preparation method according to claim 1 is characterized in that: in the step (1), the mass fraction that said p-aramid fiber condensate accounts for the p-aramid fiber polymer solution is 18 ~ 21%.
3. preparation method according to claim 1; It is characterized in that: in the step (1); The first half of two intermeshing twin-screws is that kneading piece and a spot of reverse thread cover by various forward thread bush, different rotation directions combines in the said high shear double screw extruder, and the total length of wherein mediating piece accounts for more than 30% of this partial-length.
4. preparation method according to claim 3 is characterized in that: the latter half of twin-screw is made up of the thread bush that reduces gradually along Way out pitch in the said high shear double screw extruder.
5. preparation method according to claim 1; It is characterized in that: said continuous film defoaming device be by the charging basket of jacketed, be arranged in the charging basket and and the charging basket inwall between leave the gap sector, be used to drive the transmission device of sector rotation, and the charging aperture that points to sector constitutes; And sector can form funnel with the charging basket inwall on 360 ° of directions in rotary course, makes the material that gets in the said charging basket from said charging aperture under the rotary centrifugal force effect, forming film on the sector.
6. preparation method according to claim 1 is characterized in that: in the step (5), the distance on the spinneret cap between the spray orifice is 5 ~ 10 times of injection diameter.
7. the p-aramid fiber fine count fiber that is prepared from each described preparation method in the claim 1 ~ 6; It is characterized in that: the denier range of said p-aramid fiber fine count fiber is between 30 ~ 100 dawn; TENSILE STRENGTH >=22CN/dtex; Elongation at break >=2.5%, initial modulus >=550CN/dtex.
8. the described p-aramid fiber fine count fiber of claim 7 is in the application in communication electronic equipment field.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469314A (en) * | 2013-09-13 | 2013-12-25 | 东华大学 | Method for quickly preparing PPTA (poly-paraphenylene terephthalamide) resin liquid crystal spinning solution with ultrahigh molecular weight |
| CN106544748A (en) * | 2016-11-01 | 2017-03-29 | 烟台泰和新材料股份有限公司 | A kind of high drawing p-aramid fiber filament industry production method |
| CN106906525A (en) * | 2017-03-30 | 2017-06-30 | 清华大学 | A kind of preparation method of p-aramid fiber low denier fibers long filament |
| CN112090289A (en) * | 2020-09-15 | 2020-12-18 | 苏州足迹自动化设备有限责任公司 | Device and process for preparing hollow fiber membrane by spinning hollow fiber yarns |
| CN115787124A (en) * | 2022-12-27 | 2023-03-14 | 烟台泰和新材料股份有限公司 | Preparation process of superfine denier para-aramid fiber |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103469314A (en) * | 2013-09-13 | 2013-12-25 | 东华大学 | Method for quickly preparing PPTA (poly-paraphenylene terephthalamide) resin liquid crystal spinning solution with ultrahigh molecular weight |
| CN106544748A (en) * | 2016-11-01 | 2017-03-29 | 烟台泰和新材料股份有限公司 | A kind of high drawing p-aramid fiber filament industry production method |
| CN106906525A (en) * | 2017-03-30 | 2017-06-30 | 清华大学 | A kind of preparation method of p-aramid fiber low denier fibers long filament |
| CN106906525B (en) * | 2017-03-30 | 2019-01-11 | 清华大学 | A kind of preparation method of p-aramid fiber low denier fibers long filament |
| CN112090289A (en) * | 2020-09-15 | 2020-12-18 | 苏州足迹自动化设备有限责任公司 | Device and process for preparing hollow fiber membrane by spinning hollow fiber yarns |
| CN115787124A (en) * | 2022-12-27 | 2023-03-14 | 烟台泰和新材料股份有限公司 | Preparation process of superfine denier para-aramid fiber |
| CN115787124B (en) * | 2022-12-27 | 2024-02-20 | 宁夏泰和芳纶纤维有限责任公司 | Preparation process of superfine denier para-aramid fiber |
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Application publication date: 20120711 Assignee: JIANGSU RUISHENG NEW MATERIAL TECHNOLOGY CO., LTD. Assignor: Suzhou Zhaoda Specially Fiber Technical Co., Ltd. Contract record no.: 2017320010004 Denomination of invention: Para-aramid fine denier fiber and preparation method thereof Granted publication date: 20141210 License type: Exclusive License Record date: 20170301 |
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Effective date of registration: 20190612 Address after: 210019 No. 19 Central Avenue, Yangzhou Chemical Park, Yizheng City, Yangzhou City, Jiangsu Province Patentee after: Sinochem High Performance Fiber Material Co., Ltd. Address before: 215522 No. 20 Haiping Road, New Material Industrial Park, Changshu City, Suzhou City, Jiangsu Province Patentee before: Suzhou Zhaoda Specially Fiber Technical Co., Ltd. |