CN115787124A - Preparation process of superfine denier para-aramid fiber - Google Patents
Preparation process of superfine denier para-aramid fiber Download PDFInfo
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- CN115787124A CN115787124A CN202211678966.1A CN202211678966A CN115787124A CN 115787124 A CN115787124 A CN 115787124A CN 202211678966 A CN202211678966 A CN 202211678966A CN 115787124 A CN115787124 A CN 115787124A
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- 239000000835 fiber Substances 0.000 title claims abstract description 100
- 229920003235 aromatic polyamide Polymers 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000009987 spinning Methods 0.000 claims abstract description 103
- 238000001035 drying Methods 0.000 claims abstract description 55
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 claims abstract description 49
- 239000004973 liquid crystal related substance Substances 0.000 claims abstract description 47
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 33
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 20
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 17
- WRDNCFQZLUCIRH-UHFFFAOYSA-N 4-(7-azabicyclo[2.2.1]hepta-1,3,5-triene-7-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1C2=CC=C1C=C2 WRDNCFQZLUCIRH-UHFFFAOYSA-N 0.000 claims abstract description 13
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract 9
- 239000002245 particle Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 16
- 239000000376 reactant Substances 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 claims description 7
- 230000003472 neutralizing effect Effects 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 239000004760 aramid Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 239000011550 stock solution Substances 0.000 abstract description 16
- 239000000047 product Substances 0.000 abstract description 11
- 229910001628 calcium chloride Inorganic materials 0.000 abstract description 6
- 239000001110 calcium chloride Substances 0.000 abstract description 6
- 238000007380 fibre production Methods 0.000 abstract description 2
- 239000002954 polymerization reaction product Substances 0.000 abstract 2
- 238000001125 extrusion Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 27
- 239000002585 base Substances 0.000 description 17
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 16
- 238000004090 dissolution Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 229920006231 aramid fiber Polymers 0.000 description 3
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- 238000005457 optimization Methods 0.000 description 3
- 230000001112 coagulating effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002166 wet spinning Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention provides a preparation process of superfine denier para-aramid fiber, belonging to the technical field of chemical fiber production, p-phenylenediamine is dissolved in an N-methyl pyrrolidone/calcium chloride solvent, p-phthaloyl chloride is added for the first time according to a set proportion to carry out prepolymerization reaction, the prepolymerization product is cooled, then the p-phthaloyl chloride is added for the second time according to the set proportion and enters a double-screw reactor, polymerization reaction is continuously mixed in a screw extrusion dynamic mixer to obtain a polymerization reaction product, and the polymerization reaction product is ground, neutralized, washed and dried to obtain a finished product polymer poly (p-phenylene terephthalamide PPTA); and dissolving the polymer PPTA and concentrated sulfuric acid according to a set proportion, controlling the initial dissolving temperature, finally forming liquid crystal spinning stock solution, defoaming and filtering the liquid crystal spinning stock solution, feeding the liquid crystal spinning stock solution into a spinning production line, performing spinning, washing, drying and oiling, and finally obtaining the superfine denier para-aramid fiber.
Description
Technical Field
The invention belongs to the technical field of chemical fiber production, relates to a preparation process of a para-aramid fiber, and particularly relates to a preparation process of a superfine denier para-aramid fiber.
Background
The para-aramid fiber has excellent performances of high specific strength, high specific modulus, high temperature resistance, flame retardance and the like, and is called as world three high-performance fibers together with carbon fiber and high-strength high-modulus polyethylene. The para-aramid fiber has good impact resistance, corrosion resistance and fatigue resistance.
The para-aramid fiber is generally prepared by a polymerization process, wherein poly-p-phenylene terephthamide (PPTA) powder is prepared by performing polycondensation reaction on terephthaloyl chloride (TPC) and p-phenylenediamine (PPD), then a spinning process is performed, the poly-p-phenylene terephthamide (PPTA) powder and concentrated sulfuric acid are added into a dissolving machine according to a certain proportion, and the para-aramid fiber is obtained through a spinning process.
Patent document (CN 102560700A) discloses a para-aramid fine denier fiber and a preparation method thereof, wherein a high-shear twin-screw extruder and a continuous film defoaming device are adopted, and the para-aramid fine denier fiber can be prepared by performing process integral optimization through multiple filtering processes, defoaming purity, spinning temperature, stretching conditions and the like.
Patent document (CN 106906525A) discloses a preparation method of para-aramid low-denier fiber filaments, which utilizes a spinneret to reduce the risk of extruding, overflowing and doubling aramid spinning dope, washes nascent tows with alkali liquor, quickly neutralizes sulfuric acid, further improves strength of the tows, and reduces the risk of filament breakage in a washing and drying process by adopting a flat-laying washing and drying mode. The method mainly improves the quality stability of the para-aramid low-denier fiber yarns through optimization of a tow washing process and optimization of a tow drying process. But the property of the spinning stock solution in the quality factor of the tows is not changed, so the method has certain limitation on improving the quality of the para-aramid low-denier fiber.
The difference of the spinning process of the ultra-fine denier para-aramid fiber and the common para-aramid fiber is that the number of fibers in a low-denier fiber tow is small, and the diameter of a single fiber is smaller. Therefore, the requirements of the superfine denier para-aramid fiber on the preparation process are strict, any preparation process control point influences the spinning process, any process control error causes yarn breakage, the appearance of a finished product is poor, and the use of a customer is influenced finally.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation process of superfine denier para-aramid fiber, which comprises the following steps:
s1, p-phenylenediamine is fully dissolved in an N-methylpyrrolidone/calcium chloride solution to obtain a p-phenylenediamine dissolved substance, and the mass concentration of calcium chloride in the obtained dissolved substance is 8.0% -8.6%.
S2, adding terephthaloyl chloride into the p-phenylenediamine dissolved substance obtained in the step S1 for the first time to perform a prepolymerization reaction, cooling the prepolymerization reaction, adding terephthaloyl chloride for the second time, and performing a polymerization reaction in a double-screw reactor to obtain a polymerization reactant;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthamide;
s4, adding the poly-p-phenylene terephthalamide (PPTA) powder obtained in the step S3 and concentrated sulfuric acid into a dissolving machine according to a certain proportion, controlling the reaction initial temperature, and obtaining liquid crystal spinning solution after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering and spinning;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber.
In the invention, the mass ratio of the added p-phenylenediamine to the terephthaloyl chloride is 1, and the mass ratio of the first addition of the terephthaloyl chloride to the second addition of the terephthaloyl chloride is 32-37%: 68% -63%;
the spinning process adopts a spinneret plate, the number of holes of the spinneret plate is 20-100, and the spinning monofilaments are 1D-4D para-aramid fibers.
According to the invention, the opening degree of the polymerization double-screw reactor, the ratio of p-phenylenediamine to terephthaloyl chloride and the addition mode of terephthaloyl chloride are controlled, so that the IV value of the polymer obtained in the step S2 is more than or equal to 7, and the IV value is an intrinsic viscosity value.
The polymerization reaction of the p-phenylenediamine and the terephthaloyl chloride is exothermic, so that if the terephthaloyl chloride is added at one time, the environment temperature of the polymerization reaction is sharply increased, the polymerization reaction is not favorable for completely performing the polymerization reaction of the p-phenylenediamine and the terephthaloyl chloride, the polymerization reaction is incomplete, and a large amount of side reactions are generated.
In order to realize the full dissolution of PPTA and concentrated sulfuric acid in a dissolving machine and form a smooth liquid crystal spinning solution, after a polymerization reactant is obtained in step S2, the particle size of a screen of a grinding machine is controlled, so that the proportion of the particle size of the obtained PPTA is more than 90% when the particle size of the obtained PPTA is 200-450 mu m, the particle size distribution is in normal distribution, the obtained PPTA is fine particles, if the main particle size distribution is less than 200 mu m, the PPTA is powdery, and because the specific surface area of the particles is too large, sulfuric acid cannot completely infiltrate the PPTA, the PPTA cannot be completely dissolved in the sulfuric acid, a large amount of sulfuric acid coated and agglomerated PPTA blocky particles exist in a finally formed product, and the blocky particles can influence the subsequent spinning process, such as filter blockage. When the particle size is larger than 450 μm, the PPTA particles are too large, and the PPTA particles cannot be fully contacted with sulfuric acid and completely dissolved.
In order to ensure the smooth spinning process, in the invention, the concentration of the liquid crystal spinning solution obtained in the step S4 is 19.8-20.5%, when the concentration of the liquid crystal spinning solution is too low, the strength of the filament bundle is too low, the filament breakage is serious, and when the concentration of the liquid crystal spinning solution is too high, the filament cannot be normally spun.
Because PPTA dissolution and concentrated sulfuric acid dissolution are exothermic reactions, in order to ensure the full progress of the dissolution process, the concentrated sulfuric acid concentration of the invention is 99.90-100.00%, and the initial temperature of the concentrated sulfuric acid is controlled at 15-25 ℃.
In the step S4, the dissolving process is controlled by external temperature, so that the initial reaction temperature is 10-20 ℃.
The total time of the steps S4-S5 is 4-5 h. If the total length is too long, the precipitation and delamination of PPTA and sulfuric acid in the spinning solution can be caused, and the spinning process is difficult to start. If the time is too short, on the one hand, the liquid-crystalline spinning dope is insufficiently dissolved and the spinnability is poor, and on the other hand, SO in the spinning dope 2 /SO 3 Can not remove clean SO remained in the spinning solution 2/ SO 3 The quality of the aramid fiber is influenced.
In the step S6, the temperature at the early stage of drying is 60-80 ℃, the temperature at the later stage of drying is 90-110 ℃, and the drying time is 0.5-1s. The fiber after washing contains a large amount of water, in order to control the water content of the fiber after spinning to be 3% -7% and improve the performance of the fiber, the temperature in the early stage of drying is 60-80 ℃, the water on the surface of the fiber is removed, the temperature in the later stage of drying is 90-110 ℃, the water in the middle and deep layer of the fiber is dried out, and the drying effect is further achieved. If the temperatures of the two sections are set to be 60-80 ℃, the outer layer is dried due to the fact that the fibers are of a skin-core structure, but a large amount of water is reserved in the inner layer; if the temperature of the two sections is set to be 90-110 ℃, the fiber is directly dried at high temperature, so that the surface of the fiber is badly defected, and the performance of the fiber is further influenced.
The spinning device used in the spinning process in the step S5 comprises:
the liquid crystal display panel comprises an inlet flange, a liquid crystal nozzle and a flange surface, wherein one side of the inlet flange is provided with the liquid crystal nozzle, and the other side of the inlet flange is the flange surface;
the base is connected with the flange surface of the inlet flange and comprises a base flange surface and a cavity arranged at one end of the flange surface, the cavity is in a hollow spherical shape, and an external thread surface is arranged on the outer side surface corresponding to the base cavity; spinning solution is discharged from the nozzle, enters the assembly, and then is sprayed to be connected with the clamping sleeve and the solution pipeline.
A dispersion plate is arranged at the outer side of the cavity of the base, is arranged at the outlet of the cavity and is in interference fit with the cavity; the stoste passes through the pump delivery, can produce certain pressure, and the dispersion board is with pressure dispersion, and the stable stoste flow is inside with spinning stoste evenly distributed to the cutting ferrule.
A spinneret plate coupled to the base, the spinneret plate comprising: the spinning device comprises a bottom plate, a cylinder and a spinning surface, wherein the cylinder is arranged on the bottom plate, the spinning surface is formed by the other end surface of the cylinder, filter mesh holes of the spinning surface are arranged in concentric circles, the spinning surface is a concave surface from inside to outside, and the bottom plate is a circular plate formed by the extension of the end surface of the cylinder;
the cutting ferrule is arranged on the outer side of the base, a sealing washer is directly arranged on the cutting ferrule and the spinneret circular plate, and an inner thread surface matched with the base is arranged on the inner liner of the cutting ferrule.
Aiming at the superfine denier para-aramid fiber, the spinneret plate 33 and the spinneret plate 66 with holes are selected to spin the 1-4D superfine denier para-aramid fiber by the corresponding spinneret device.
Because the wet spinning process is sprayed dry, rely on the rivers in the coagulating bath tray, prepare the nascent fibre, under the general condition, the falling velocity of the liquid crystal state stock solution of the midmost is greater than the falling velocity of liquid crystal state stock solution all around, consequently can lead to the liquid crystal body in the spinneret to spout the silk inhomogeneous, in order to solve this problem, this application sets the spinneret into the concave surface, thereby shortened the time difference that middle liquid crystal state stock solution and liquid crystal state stock solution all around spout the silk, it receives the influence of process to reduce the liquid crystal state stock solution blowout speed in the spinning device, can spout the silk evenly.
The invention also provides the superfine denier para-aramid fiber obtained by the preparation process of the superfine denier para-aramid fiber, the superfine denier para-aramid fiber has a flat appearance, the fiber denier is 1-4D, the linear density deviation rate is less than 3%, the breaking strength is more than or equal to 18cN/dtex, the elongation at break is 2% -4%, the initial modulus is 70-110Gpa, and the number of broken filaments is less than or equal to 8 per 2kg. The unit of the number of the filaments can also be a unit/cylinder of the requirement of the appearance project of the para-aramid filament yarn in a para-aramid filament yarn (Q/0601 THX004-2017) which is filed in an enterprise standard information public service platform (https:// www.qybz.org.cn /) by Futaitaitai and new material stock Co., 12.12.28.09 points and 50 points, namely the number of the filaments of the ultra-fine denier para-aramid fiber is less than or equal to 8 per cylinder.
The invention has the outstanding technical effects that:
the polymerization reaction of the p-phenylenediamine and the terephthaloyl chloride is exothermic, so if the p-phthaloyl chloride is added at one time, the environment temperature of the polymerization reaction is sharply increased, the polymerization reaction is not favorable for completely performing the polymerization reaction of the p-phenylenediamine and the terephthaloyl chloride, the polymerization reaction is incomplete, and a large amount of byproducts are generated.
The method controls the particle size of PPTA, is favorable for obtaining the spinning stock solution in the optimal state, increases the fluidity and smoothness of the stock solution, and reduces small lumps of fine sulfuric acid coated powder.
The exothermic reaction is carried out in the mixing process of the PPTA and the concentrated sulfuric acid, the jacket is arranged on the feeding screw rod by adding the external cooling system, heat is rapidly taken away through low-temperature circulating water when the PPTA and the concentrated sulfuric acid are mixed, the initial reaction temperature is controlled to be 10-20 ℃, the heat generated in the mixing process of the PPTA and the concentrated sulfuric acid is taken away, the formation of liquid crystal solution in the mixing and dissolving process of the PPTA and the concentrated sulfuric acid can be promoted, and the problem that the PPTA and the concentrated sulfuric acid are not fully dissolved to form PPTA agglomerated hard blocks due to the fact that the PPTA and the concentrated sulfuric acid are not fully dissolved in the violent heat reaction dissolving process is solved.
The time from the dissolving preparation to the whole process of spinning ejection is set to be 4h-5h, so that the stock solution residence time is set to be 4h-5h, the spinning stock solution is ensured to be in a liquid crystal state, and if the spinning liquid crystal solution residence time is too long, the settling and layering of PPTA and sulfuric acid in the spinning stock solution can be caused, the spinning process is difficult to start, and the fiber strength is reduced. If the time is too short, insufficient dissolution of the liquid-crystalline spinning dope may occur on the one hand, and SO in the spinning dope may occur on the other hand 2 /SO 3 Can not remove clean SO remained in the spinning solution 2 /SO 3 The S content of the aramid fiber is not increased, and the performance of the fiber is not influenced. The dissolving time is controlled to obtain liquid crystal spinning solution with optimal fluidity, which is favorable for spinning fine denier fibers.
Because the wet spinning process of dry-jet, rely on the rivers in the coagulating bath tray, prepare the nascent fibre, under the general condition, the falling velocity of the liquid crystal state stoste of the midmost is greater than the falling velocity of liquid crystal state stoste all around, consequently can lead to the liquid crystal in the spinneret to spout the silk inhomogeneous, in order to solve this problem, this application sets the spinneret into the concave surface, thereby shortened the time difference that middle liquid crystal state stoste and liquid crystal state stoste all around spout the silk, it receives the influence of spinning technology to reduce the liquid crystal state stoste blowout speed in the spinning device, can spout the silk evenly. The appearance of the superfine denier fiber is easy to generate defects such as broken filaments and the like, and the use of customers is influenced, so that the defects caused by equipment can be effectively avoided by using clean water for washing and reducing tension rollers.
Drawings
FIG. 1 is an isometric view of a spinning apparatus;
FIG. 2 is a top plan view of an isometric view of a spinning apparatus;
FIG. 3 is a sectional view taken along plane A of FIG. 2;
in the figure, an inlet flange 100, a liquid crystal nozzle 101, a flange face 102; the spinning nozzle comprises a base 200, a base flange face 201, a cavity 201, an external thread face 203, a dispersion plate 300, a spinneret plate 400, a bottom plate 401, a cylinder 402, a spinning face 403, a sealing washer 500, a clamping sleeve 600 and an internal thread face 601.
Detailed Description
The following examples and comparative examples further illustrate the present invention in detail.
The preparation process of the superfine denier para-aramid fiber comprises the following steps:
s1, p-phenylenediamine is fully dissolved in an N-methylpyrrolidone/calcium chloride solution to obtain a p-phenylenediamine dissolved substance;
s2, adding paraphthaloyl chloride into the p-phenylenediamine dissolved substance obtained in the step S1 for the first time to perform prepolymerization reaction, cooling the prepolymerization reaction, adding paraphthaloyl chloride for the second time, and performing polymerization reaction in a double-screw reactor to obtain a polymerization reactant;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthalamide;
s4, dissolving the poly-p-phenylene terephthalamide obtained in the step S3 and concentrated sulfuric acid in a dissolving machine according to a certain ratio, controlling the initial reaction temperature, and obtaining liquid crystal spinning solution after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering and spinning;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber.
The mass ratio of the added phenylenediamine to the terephthaloyl chloride is 1, and the mass ratio of the terephthaloyl chloride added for the first time to the terephthaloyl chloride added for the second time is 32-37%: 68% -63%;
the spinning process adopts a spinneret plate, the number of holes of the spinneret plate is 20-100, and the spinning monofilaments are 1D-4D para-aramid fibers.
The IV value of the polymer obtained in the step S2 is not less than 7.
In the step S3, the particle size of 80 percent of PPTA obtained by controlling the particle size of a screen of a grinding machine is 200-450 mu m.
The concentration of the liquid crystal spinning solution obtained in the step S4 is 19.8-20.5%;
in the step S4, the concentration of concentrated sulfuric acid is 99.9-100%, and the initial temperature of the concentrated sulfuric acid is controlled to be 15-25 ℃;
in the step S4, the dissolving process is controlled by external temperature, so that the initial reaction temperature is 10-20 ℃;
in the step S5, the size of a filter screen in the filter is 3-10 μm;
the total time of the steps S4 to S5 is 4-5 h;
in the step S6, the temperature at the early stage of drying is 60-80 ℃, the temperature at the later stage of drying is 90-110 ℃, and the drying time at the early stage of drying and the drying time at the later stage of drying are both 0.5-1s.
The specific embodiments of the present application are as follows:
example 1
Continuously introducing p-phenylenediamine into the reaction system of S1, dissolving the p-phenylenediamine in an N-methylpyrrolidone/calcium chloride solution, fully and uniformly mixing to obtain a p-phenylenediamine dissolved substance, and controlling the introduction amount of the p-phenylenediamine and the N-methylpyrrolidone/calcium chloride solution to enable the mass concentration of calcium chloride in the p-phenylenediamine dissolved substance to be 8.0-8.3%;
s2, adding 32% of terephthaloyl chloride into the p-phenylenediamine dissolved substance obtained in the step S1 for the first time to perform a prepolymerization reaction, cooling the prepolymerization to 5-6 ℃, adding 68% of terephthaloyl chloride for the second time, wherein the mass ratio of the total amount of the terephthaloyl chloride added for the two times to the p-phenylenediamine dissolved substance obtained in the step S1 is 1:1; carrying out polymerization reaction in a double-screw reactor to obtain a polymerization reactant, wherein the IV value of the obtained polymer is 7.4 in the step;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthalamide PPTA, wherein the particle size of a screen of the grinding machine is controlled in the step, and the particle size of 90% of the obtained PPTA is 200-450 mu m;
s4, dissolving the finished polymer poly-p-phenylene terephthalamide obtained in the step S3 and concentrated sulfuric acid with the concentration of 99.9% in a dissolving machine, controlling the initial reaction temperature to be 25 ℃, controlling the external temperature to be 20 ℃, and controlling the adding amount of the concentrated sulfuric acid to obtain a liquid crystal spinning solution with the concentration of 19.8% after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering, and performing spinning, wherein the size of a filter screen is 3 mu m, a spinneret plate is adopted in the spinning process, the number of holes of the spinneret plate is 100, and 1D of spun monofilaments are adopted;
the total time length of the steps S4-S5 is 4h;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber, wherein the temperature at the early stage of drying is 80 ℃, the drying time is 0.5S, the temperature at the later stage is 110 ℃, and the drying time is 0.5S.
The material performance of the superfine denier para-aramid fiber obtained in the embodiment is detected, and the linear density deviation rate of the obtained fiber is 2.4%, the breaking strength is 22.51cN/dtex, and the elongation at break is 3.2%; the initial modulus was 82Gpa.
Example 2
Continuously introducing phenylenediamine into the reaction system of S1, dissolving the phenylenediamine in an N-methylpyrrolidone/calcium chloride solution, fully and uniformly mixing to obtain a mixture, and controlling the introduction amount of the phenylenediamine and the N-methylpyrrolidone/calcium chloride solution to enable the mass concentration of calcium chloride in the phenylenediamine solute to be 8.2% -8.4%;
s2, adding 34% of terephthaloyl chloride into the phenylenediamine dissolved substance obtained in the step S1 for the first time to perform a prepolymerization reaction, cooling the prepolymerization to 6-7 ℃, adding 66% of terephthaloyl chloride for the second time, wherein the mass ratio of the total amount of the terephthaloyl chloride added for the two times to the p-phenylenediamine dissolved substance obtained in the step S1 is 1:1, carrying out polymerization reaction in a double-screw reactor to obtain a polymerization reactant; the IV value of the polymer obtained is 7.2;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthalamide PPTA, wherein the particle size of a screen of the grinding machine is controlled in the step, and the particle size of 90% of the obtained PPTA is 200-450 mu m;
s4, dissolving the finished polymer poly (p-phenylene terephthalamide) PPTA obtained in the step S3 and concentrated sulfuric acid with the concentration of 100% in a dissolving machine, controlling the initial reaction temperature to be 15 ℃, controlling the external temperature to enable the initial reaction temperature to be 10 ℃, and controlling the adding amount of the concentrated sulfuric acid to obtain liquid crystal spinning stock solution with the concentration of 20.0% after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering, and performing spinning, wherein the size of a filter screen is 8 mu m, a spinneret plate is adopted in the spinning process, the number of holes of the spinneret plate is 50, and the number of spun monofilaments is 2D;
the total time length of the steps S4-S5 is 5h;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber, wherein the temperature at the early stage of drying is 80 ℃, the drying time is 0.75S, the temperature at the later stage is 110 ℃, and the drying time is 0.6S.
The material performance of the superfine denier para-aramid fiber obtained in the embodiment is detected, and the obtained fiber has the linear density deviation rate of 1.8%, the breaking strength of 23.84cN/dtex, and the elongation at break of 3.4%; the initial modulus was 95GPa.
Example 3
Continuously introducing phenylenediamine into the reaction system of S1, dissolving the phenylenediamine in an N-methylpyrrolidone/calcium chloride solution, fully and uniformly mixing to obtain a mixture, and controlling the introduction amount of the phenylenediamine and the N-methylpyrrolidone/calcium chloride solution to enable the mass concentration of calcium chloride in the phenylenediamine solute to be 8.3% -8.5%;
s2, adding 35% of terephthaloyl chloride into the phenylenediamine dissolved substance obtained in the step S1 for the first time to perform a prepolymerization reaction, cooling the prepolymerization to 7-8 ℃, adding 65% of terephthaloyl chloride for the second time, wherein the mass ratio of the total amount of the terephthaloyl chloride added twice to the p-phenylenediamine dissolved substance obtained in the step S1 is 1:1, and carrying out polymerization reaction in a double-screw reactor to obtain a polymer IV value of 7.3;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product of poly-p-phenylene terephthalamide PPTA, wherein the particle size of a screen of the grinding machine is controlled in the step, and the particle size of 90% of the obtained poly-p-phenylene terephthalamide PPTA is 200-450 microns;
s4, dissolving the finished polymer poly-p-phenylene terephthalamide obtained in the step S3 and concentrated sulfuric acid with the concentration of 99.9% in a dissolving machine, controlling the initial reaction temperature to be 20 ℃, controlling the external temperature to be 15 ℃, and controlling the adding amount of the concentrated sulfuric acid to obtain liquid crystal spinning stock solution with the concentration of 20.2% after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering, and performing spinning, wherein the size of a filter screen is 10 mu m, a spinneret plate is adopted in the spinning process, the number of holes of the spinneret plate is 20, and the number of spun monofilaments is 4D;
the total time length of the steps S4-S5 is 4.5h;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber, wherein the early-stage drying temperature is 70 ℃, the drying time is 0.8S, the later-stage drying temperature is 100 ℃, and the drying time is 0.8S.
The material performance of the superfine denier para-aramid fiber obtained in the embodiment is detected, and the linear density deviation rate of the fiber is 2.1%, the breaking strength is 23.57cN/dtex, and the elongation at break is 3.5%; the initial modulus was 83 GPa.
In the above embodiment 3, the spinning device used in the spinning process in the step S5 includes: the liquid crystal display panel comprises an inlet flange 100, a liquid crystal nozzle 101 is arranged on one side of the inlet flange, and a flange surface 102 is arranged on the other side of the inlet flange; the base 200 is connected with the flange surface of the inlet flange, the base 200 comprises a base flange surface 201 and a cavity 201 arranged at one end of the flange surface, the cavity is in a hollow spherical shape, and an external thread surface 203 is arranged on the outer side surface corresponding to the base cavity; a dispersion plate 300 is arranged on the outer side of the cavity of the base, is arranged at the outlet of the cavity and is in interference fit with the cavity; a spinneret plate 400 coupled to the base, the spinneret plate comprising: the spinning device comprises a bottom plate 401, a cylinder 402 arranged on the bottom plate, and a spinning surface 403 formed by the other end surface of the cylinder, wherein filter mesh holes of the spinning surface are arranged in concentric circles, the spinning surface is a concave surface from inside to outside, and the bottom plate is a circular plate formed by the extension of the end surface of the cylinder; the cutting ferrule 600 that sets up in the base outside, cutting ferrule and spinneret plectane directly set up seal ring 500, the cutting ferrule inside lining sets up and base complex internal thread face 601.
The spinning device is utilized to set different specifications for spinning, and the physical indexes are as shown in the following table 1:
example 4
Continuously introducing phenylenediamine into the reaction system of S1, dissolving the phenylenediamine in an N-methylpyrrolidone/calcium chloride solution, fully and uniformly mixing to obtain a mixture, and controlling the introduction amount of the phenylenediamine and the N-methylpyrrolidone/calcium chloride solution to enable the mass concentration of calcium chloride in the phenylenediamine dissolved substance to be 8.4% -8.6%;
s2, adding 37% of terephthaloyl chloride into the phenylenediamine dissolved substance obtained in the step S1 for the first time to perform a prepolymerization reaction, cooling the prepolymerization to 8-10 ℃, adding 63% of terephthaloyl chloride for the second time, wherein the mass ratio of the total amount of the terephthaloyl chloride added for the two times to the p-phenylenediamine dissolved substance obtained in the step S1 is 1:1, and carrying out polymerization reaction in a double-screw reactor to obtain a polymer IV value of 7.3;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthamide (PPTA), wherein the particle size of a screen of the grinding machine is controlled in the step, and the particle size of 90% of the obtained poly-p-phenylene terephthamide (PPTA) is 200-450 mu m;
s4, dissolving the finished product polymer poly-p-phenylene terephthamide obtained in the step S3 and concentrated sulfuric acid with the concentration of 100% in a dissolving machine, controlling the initial reaction temperature to be 20 ℃, controlling the external temperature to enable the initial reaction temperature to be 15 ℃, and controlling the adding amount of the concentrated sulfuric acid to obtain a liquid crystal spinning solution with the concentration of 20.5% after the dissolution is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering, and performing spinning, wherein the size of a filter screen is 10 mu m, a spinneret plate is adopted in the spinning process, the number of holes of the spinneret plate is 20, and the number of spun monofilaments is 4D;
the total time length of the steps S4-S5 is 4.5h;
and S6, washing and drying the para-aramid fiber spun in the step S5 to obtain the superfine denier para-aramid fiber, wherein the early-stage drying temperature is 60 ℃, the drying time is 1S, the later-stage drying temperature is 90 ℃, and the drying time is 1S.
The material performance of the superfine denier para-aramid fiber obtained in the embodiment is detected, and the linear density deviation rate of the fiber is 2.2%, the breaking strength is 22.58cN/dtex, and the elongation at break is 3.5%; the initial modulus was 81 GPa.
Comparative example 1
The difference between the comparative example and the example 3 is that in the step S2, all terephthaloyl chloride is added once and then prepolymerization is carried out, the other steps and control parameters are the same as those in the example 3, and the IV value of the obtained polymer is 6.8;
the material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 2.8 percent, the breaking strength is 18.23cN/dtex, and the elongation at break is 2.8 percent; the initial modulus was 81 GPa.
Comparative example 2
The difference between the comparative example and the example 3 is only that in the step S3, the particle size of the screen of the grinding machine is controlled, and the particle size 90 percent distribution of the obtained poly-p-phenylene terephthalamide PPTA is 130-200 mu m; the other steps and control parameters were the same as in example 3.
Under the condition that other parameters are not changed, the sulfuric acid cannot completely infiltrate the PPTA due to the excessively low particle size, and small lumps of the sulfuric acid coated powder are formed.
Comparative example 3
The comparative example differs from example 3 only in that in step S3, the particle size of the screen of the grinding machine is controlled, and 90% of the particle size of PPTA obtained is 450-550 μm; the other steps and control parameters were the same as in example 3. Under the condition that other parameters are not changed, when the particle size is larger than 450 mu m, the PPTA particles are too large, so that the interior of the PPTA particles can not be contacted with sulfuric acid and can not be completely dissolved.
Comparative example 4
This comparative example is different from example 3 only in that in step S4, the temperature control of the reaction vessel is not performed, and other steps and control parameters are the same as those of example 3,
as the dissolution reaction of PPTA in sulfuric acid is exothermic, and the temperature is not controlled externally, the problem that PPTA and sulfuric acid are not fully dissolved to cause that PPTA is not fully dissolved to form PPTA agglomerate hard blocks is caused.
Comparative example 5
The comparative example is different from example 3 only in that the total time of steps S4 to S5 is 3.5h, other steps and control parameters are the same as example 3,
the material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 3.2 percent, the breaking strength is 17.24 cN/dtex, and the elongation at break is 2.8 percent; the initial modulus was 73GPa.
Too short a reaction time results in insufficient dissolution of the liquid-crystalline spinning dope on the one hand and SO in the spinning dope on the other hand 2 Can not remove clean SO remained in the spinning solution 2 The quality of the aramid fiber is influenced,
comparative example 6
The comparative example is different from example 3 only in that the total time of steps S4 to S5 is 5.5h, other steps and control parameters are the same as example 3,
and (3) detecting the material performance of the superfine denier para-aramid fiber obtained by the comparative example to obtain the fiber with the linear density deviation rate of 4.3%.
The spinning liquid crystal solution has too long retention time, which causes the settling and layering of PPTA and sulfuric acid in the spinning solution, large deviation of fiber linear density and low fiber strength.
The material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 6.2 percent, the breaking strength is 10.76 cN/dtex, and the elongation at break is 3.4 percent; the initial modulus was 50GPa.
Comparative example 7
The comparative example is different from example 3 only in that the drying temperature of the fiber after water washing is set to 70 ℃ in the step S6, the drying time is 1.5S, other steps and control parameters are the same as those of example 3,
the material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 3.2%, the breaking strength is 20.33cN/dtex, and the elongation at break is 2.5%; the initial modulus was 73GPa.
Comparative example 8
This comparative example is different from example 3 only in that the drying temperature after the fiber washing in step S6 was set to 100 ℃ and the drying time was 1S, the other steps and control parameters were the same as those of example 3,
the material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 3.3 percent, the breaking strength is 21.31cN/dtex, and the elongation at break is 2.3 percent; the initial modulus was 82Gpa.
Comparative example 9
This comparative example differs from example 3 only in that in step S6, the temperature at the early stage of drying was 50 ℃, the drying time was 1S, the temperature at the late stage of drying was 120 ℃, and the drying time was 0.5S.
Other steps and control parameters were the same as in example 3,
the material performance of the superfine denier para-aramid fiber obtained by the comparative example is detected, and the linear density deviation rate of the fiber is 4 percent, the breaking strength is 21.97cN/dtex, and the elongation at break is 2 percent; the initial modulus was 73GPa.
Table 2 shows the performance indexes of the fiber materials obtained in the different examples and comparative examples.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation process of superfine denier para-aramid fiber is characterized by comprising the following steps:
s1, fully dissolving p-phenylenediamine in an N-methylpyrrolidone/calcium chloride solution to obtain a p-phenylenediamine dissolved substance;
s2, adding paraphthaloyl chloride into the p-phenylenediamine dissolved substance obtained in the step S1 for the first time to perform prepolymerization reaction, cooling the prepolymerization reaction, adding paraphthaloyl chloride for the second time, and performing polymerization reaction in a double-screw reactor to obtain a polymerization reactant;
s3, grinding, neutralizing, washing and drying the polymerization reactant obtained in the step S2 to obtain a finished product polymer poly-p-phenylene terephthalamide PPTA;
s4, adding the poly-p-phenylene terephthamide obtained in the step S3 and concentrated sulfuric acid into a dissolving machine for dissolving, controlling the initial reaction temperature, and obtaining liquid crystal spinning solution after the dissolving is finished;
s5, defoaming the liquid crystal spinning solution obtained in the step S4, filtering and spinning;
s6, washing and drying the para-aramid fiber spun in the step S5 to obtain superfine denier para-aramid fiber;
the mass ratio of the added p-phenylenediamine to the terephthaloyl chloride is 1, and the mass ratio of the terephthaloyl chloride added for the first time to the terephthaloyl chloride added for the second time is 32-37%: 68% -63%;
the spinning process adopts a spinneret plate, the number of holes of the spinneret plate is 20-100, and the spinning monofilaments are 1D-4D para-aramid fibers.
2. The process for preparing the ultra-fine denier para-aramid fiber according to claim 1, wherein the intrinsic viscosity IV value of the polymer obtained in the step S2 is not less than 7.
3. The process for preparing a super fine denier para-aramid fiber as claimed in claim 1, wherein in step S3, the particle size of the obtained polymer poly-p-phenylene terephthalamide is controlled to be in the range of 200 μm to 450 μm by controlling the particle size of the screen of the grinding machine.
4. The process for preparing the superfine denier para-aramid fiber according to claim 1, wherein the concentration of the liquid crystalline spinning solution obtained by fully dissolving the poly (p-phenylene terephthalamide) and concentrated sulfuric acid in the step S4 is 19.8-20.5%.
5. The process for preparing the ultra-fine denier para-aramid fiber according to claim 1, wherein the dissolving process of the step S4 is controlled by external temperature to make the initial reaction temperature be 10 ℃ to 20 ℃;
the preparation process of the superfine denier para-aramid fiber as claimed in claim 1, wherein the total time of the steps S4 to S5 is 4h-5h.
6. The process for preparing the ultra-fine denier para-aramid fiber according to claim 1, wherein in the step S5, the diameter of the filter screen is 3 μm to 10 μm, and the adjustment is made according to the fiber denier.
7. The process for preparing the superfine denier para-aramid fiber according to claim 1, wherein the total time of the steps S4 to S5 is 4-5 h.
8. The process for preparing the ultra-fine denier para-aramid fiber according to claim 1, wherein in the step S6, the temperature at the early stage of drying is 60-80 ℃, the temperature at the later stage of drying is 90-110 ℃, and the drying time is 0.5-1s.
9. The process for preparing the ultra-fine denier para-aramid fiber according to claim 1, wherein the spinning device used in the spinning process in the step S5 comprises:
the liquid crystal display panel comprises an inlet flange (100), wherein one side of the inlet flange is provided with a liquid crystal nozzle (101), and the other side of the inlet flange is a flange surface (102);
the base (200) is connected with the flange face of the inlet flange, the base (200) comprises a base flange face (201) and a cavity (201) arranged at one end of the flange face, the cavity is in a hollow spherical shape, and an external thread face (203) is arranged on the outer side face corresponding to the cavity of the base;
a dispersion plate (300) is arranged on the outer side of the cavity of the base, is arranged at the outlet of the cavity and is in interference fit with the cavity;
a spinneret plate (400) coupled to the base, the spinneret plate comprising: the spinning device comprises a bottom plate (401), a cylinder (402) arranged on the bottom plate, and a spinning surface (403) formed by the other end surface of the cylinder, wherein filter mesh holes of the spinning surface are arranged in concentric circles, the spinning surface is a concave surface from inside to outside, and the bottom plate is a circular plate formed by the extension of the end surface of the cylinder;
the cutting ferrule (600) is arranged on the outer side of the base, the cutting ferrule and the spinneret plate circular plate are directly provided with a sealing washer (500), and the cutting ferrule liner is provided with an inner thread surface (601) matched with the base.
10. The superfine denier para-aramid fiber obtained by the preparation process of the superfine denier para-aramid fiber according to any one of claims 1 to 9, characterized in that the superfine denier para-aramid fiber has a flat appearance, the fiber filament denier is 1D-4D, the linear density deviation rate is less than 3%, the breaking strength is more than or equal to 18cN/dtex, the elongation at break is 2% -4%, the initial modulus is 70-110Gpa, and the number of filaments is less than or equal to 8/2 kg.
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