CN117966512B - Special paper, preparation method and application - Google Patents
Special paper, preparation method and application Download PDFInfo
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- CN117966512B CN117966512B CN202410345606.2A CN202410345606A CN117966512B CN 117966512 B CN117966512 B CN 117966512B CN 202410345606 A CN202410345606 A CN 202410345606A CN 117966512 B CN117966512 B CN 117966512B
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- fiber
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- special paper
- chopped
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000835 fiber Substances 0.000 claims abstract description 507
- 238000009987 spinning Methods 0.000 claims abstract description 89
- 238000004537 pulping Methods 0.000 claims abstract description 66
- 238000001035 drying Methods 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 42
- 238000005520 cutting process Methods 0.000 claims abstract description 39
- 238000010009 beating Methods 0.000 claims abstract description 27
- 238000007731 hot pressing Methods 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims description 164
- 239000000243 solution Substances 0.000 claims description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 39
- 229920000642 polymer Polymers 0.000 claims description 39
- 239000007864 aqueous solution Substances 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 238000005098 hot rolling Methods 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 239000004751 flashspun nonwoven Substances 0.000 claims description 32
- 229920000728 polyester Polymers 0.000 claims description 31
- 238000003851 corona treatment Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 229920001230 polyarylate Polymers 0.000 claims description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 22
- 239000001301 oxygen Substances 0.000 claims description 22
- 229910052760 oxygen Inorganic materials 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 22
- 229920001474 Flashspun fabric Polymers 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000004513 sizing Methods 0.000 claims description 20
- 238000001704 evaporation Methods 0.000 claims description 19
- 230000008020 evaporation Effects 0.000 claims description 19
- 229920005594 polymer fiber Polymers 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 238000009832 plasma treatment Methods 0.000 claims description 18
- 230000006837 decompression Effects 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000004090 dissolution Methods 0.000 claims description 15
- ICXAPFWGVRTEKV-UHFFFAOYSA-N 2-[4-(1,3-benzoxazol-2-yl)phenyl]-1,3-benzoxazole Chemical compound C1=CC=C2OC(C3=CC=C(C=C3)C=3OC4=CC=CC=C4N=3)=NC2=C1 ICXAPFWGVRTEKV-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000004806 packaging method and process Methods 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000011162 core material Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 150000008282 halocarbons Chemical class 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- 229920000098 polyolefin Polymers 0.000 claims description 3
- 238000007639 printing Methods 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 claims description 3
- 230000001954 sterilising effect Effects 0.000 claims description 3
- 238000004659 sterilization and disinfection Methods 0.000 claims description 3
- 238000004078 waterproofing Methods 0.000 claims description 3
- -1 alicyclic hydrocarbon Chemical class 0.000 description 87
- 239000004698 Polyethylene Substances 0.000 description 85
- 229920000573 polyethylene Polymers 0.000 description 85
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 30
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 30
- 229920003235 aromatic polyamide Polymers 0.000 description 25
- 239000004696 Poly ether ether ketone Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 24
- 229920002530 polyetherether ketone Polymers 0.000 description 24
- 239000004760 aramid Substances 0.000 description 22
- 230000000630 rising effect Effects 0.000 description 22
- 229920000747 poly(lactic acid) Polymers 0.000 description 21
- 239000004626 polylactic acid Substances 0.000 description 21
- 238000001914 filtration Methods 0.000 description 17
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 13
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 10
- 238000005507 spraying Methods 0.000 description 10
- 229920000927 poly(p-phenylene benzobisoxazole) Polymers 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 240000006677 Vicia faba Species 0.000 description 3
- 235000010749 Vicia faba Nutrition 0.000 description 3
- 235000002098 Vicia faba var. major Nutrition 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000001112 coagulating effect Effects 0.000 description 3
- 229960005215 dichloroacetic acid Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 206010061592 cardiac fibrillation Diseases 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000011557 critical solution Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002600 fibrillogenic effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000008041 oiling agent Substances 0.000 description 2
- 229920001432 poly(L-lactide) Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920001470 polyketone Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 2
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 1
- 206010066054 Dysmorphism Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229920004695 VICTREX™ PEEK Polymers 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
Landscapes
- Paper (AREA)
Abstract
The invention provides special paper, a preparation method and application thereof, and belongs to the technical field of special paper, wherein the special paper comprises at least two kinds of fibers, contains pulp fibers accounting for 10-80 wt% of the total weight of the special paper, and contains chopped fibers accounting for 10-90 wt% of the total weight of the special paper; the pulp fiber is prepared by flash spinning, more than 50% of the pulp fiber has at least two branches on the length of 1mm, the beating degree is 10-80 DEG SR after cutting, pulping and beating, the length of the chopped fiber is 3-10 mm, the fiber denier is 1-3D, and the special paper is prepared by wet papermaking, squeezing, drying and hot pressing treatment after mixing. The pulp fiber prepared by flash spinning and the chopped fiber are organically combined to prepare the special paper with high peel strength and puncture strength.
Description
Technical Field
The invention belongs to the technical field of special paper, and particularly relates to special paper, a preparation method and application.
Background
Compared with plant fibers, the polymer fibers not only have higher mechanical properties, but also have the characteristics of polymer bodies, such as flame retardance, insulation, corrosion resistance, antibacterial property, high temperature resistance, weather resistance and the like. The polymer fiber paper is widely used for paper making such as wallpaper, bond paper, insulating paper, filter paper, dust-free paper and the like.
The current methods for preparing pulp from polymer fibers mainly comprise a fiber beating method and a phase conversion method. For example, polymer fibers are prepared by melt spinning or solution spinning, chopped fibers are prepared by cutting long fibers, the chopped fibers are subjected to mechanical pulping treatment, and the fibers are subjected to filament splitting and fibrillation to obtain pulp fibers; injecting the resin solution into a coagulating bath, and precipitating to obtain fibrids after high-speed centrifugal shearing. The short fiber pulping method has low fiber beating degree and poor dispersion, and needs beating treatment when in use, and has poor mechanical property after paper formation. The phase conversion method has strict requirements on equipment rotation speed, solution property and precipitant property, and the fiber prepared by the method has poor uniformity, low crystallinity, large thermal shrinkage after paper forming and contains small nodes or small hard blocks without film formation.
The surface of the polymer fiber lacks hydrophilic functional groups, so that the surface energy of the polymer fiber is low, the dispersion performance in aqueous solution is poor, and the wet papermaking performance is poor.
The flash spinning technology is that the polymer and the solvent form spinning solution under high temperature and high pressure, and the solvent flash flashes rapidly after the spinning solution passes through a decompression nozzle to obtain the fiber spinning technology. The flash spun fiber is continuous long fiber, has a small diameter, a large diameter distribution range of about 0.1-10um and high crystallinity, but is endless continuous long fiber, and the long fiber is difficult to prepare paper or non-woven fabric sheet directly by wet papermaking technology.
Disclosure of Invention
In order to solve the problems, the invention provides special paper, a preparation method and application. The pulp fiber prepared by flash spinning and the chopped fiber are organically combined to prepare the special paper with high peel strength and puncture strength.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The invention provides special paper, which comprises at least two types of fibers, wherein the pulp fibers comprise 10-80 wt% of the total weight of the special paper, and the chopped fibers comprise 10-90 wt% of the total weight of the special paper; the pulp fiber is prepared by flash spinning, more than 50% of the pulp fiber has at least two branches on the length of 1mm, the beating degree is 10-80 DEG SR after cutting, pulping and beating, the length of the chopped fiber is 3-10 mm, the fiber denier is 1-3D, and the special paper is prepared by wet papermaking, squeezing, drying and hot pressing treatment after mixing.
Further, the diameter range of the pulp fiber is 0.1-18 mu m, wherein 80% of the diameter range is 5-10 mu m, the length after cutting is 0.1-20.0 mm, and the particle size ratio of the pulp fiber is less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1.
Further, the pulp fiber has a profile of 20% -80%.
Further, the mass ratio of the pulp fiber to the chopped fiber is 1: (1.2 to 1.5).
Further, the degree of irregularity of the chopped fibers is 30-80%.
The invention provides a preparation method of the special paper, which comprises the following steps: preparing pulp fiber slurry; preparing a chopped fiber slurry; pulping the pulp fiber slurry and the chopped fiber slurry respectively, mixing the pulp fiber slurry and the chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
Further, preparing a pulp fiber slurry includes: adding a polymer and a solvent R1 into a reaction kettle, controlling the temperature of the reaction kettle to be higher than an upper critical dissolution temperature for at least 1min, then reducing the temperature to be lower than the upper critical dissolution temperature for 1-600 s at a cooling rate of at least 5 ℃/min, increasing the temperature to be higher than the upper critical dissolution temperature for 6-600 s at a heating rate of at least 5 ℃/min, repeating the temperature reducing and heating processes, maintaining the pressure to be at least 3Mpa, and preparing flash spinning fibers in a flash evaporation mode;
Or adding the polymer and the solvent R1 into a reaction kettle, controlling the pressure of the reaction kettle to be higher than the cloud point pressure for at least 1min, then reducing the pressure to be lower than the cloud point pressure for 60-2000 s at a reducing speed of at least 0.05MPa/min, increasing the pressure to be higher than the cloud point pressure for 60-2000 s at a increasing speed of at least 0.05MPa/min, repeating the reducing and increasing processes, maintaining the temperature to be higher than at least the upper critical dissolution temperature, and preparing the flash spinning fiber through a flash evaporation mode;
cutting the flash spinning fiber to 0.1-20 mm, and pulping to obtain pulp fiber with a beating degree of 10-80 DEG SR; and after drying, carrying out hydrophilic treatment on the pulp fiber to obtain the modified pulp.
Further, the pulping treatment process comprises the following steps: adding deionized water to defibering for 5-50 min, wherein the slurry concentration during pulping is 0.01-0.1wt%, feeding a heavy cutter to defibering for 1-10 min, feeding a light cutter to defibering for 30-200 min.
Further, the polymer comprises polyolefin, polyester, polyether ether ketone and polyketone with melting points, and meta-aramid, para-aramid, polyarylate, poly-p-phenylene benzobisoxazole and polyimide without melting points; the solvent R1 is one or more of water, alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halogenated hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, aromatic hydrocarbon and unsaturated hydrocarbon; the temperature and pressure in the reaction kettle are controlled by an auxiliary gas and a heating system cooling system, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
Further, the flash evaporation mode is that polymer spinning solution is sprayed into nitrogen with the temperature of 50-500 ℃ through a decompression nozzle of flash evaporation spinning equipment; or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polymer through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70wt%.
Further, cutting the flash spun fiber to 0.1-20 mm comprises: cutting off the flash spun fibers to obtain four kinds of length fibers with the length ranges of 0.1-0.4 mm, 2.5-3.5 mm, 9.5-10.5 mm and 18-20 mm respectively, and mixing the flash spun chopped fibers with the same mass and four kinds of length.
Further, preparing the chopped fiber slurry includes: and carrying out hydrophilic treatment on the chopped fibers with the length of 3-10 mm, the fiber denier of 1-3D and the profile degree of 30-80%.
Further, the hydrophilic treatment is to increase the surface energy of the fibers to at least 38 mN/m.
Further, the hydrophilic treatment is corona treatment, and the corona treatment process is as follows: the voltage of corona treatment is 4000-16000V, the frequency is 12-26 KHz, the distance between an electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h; or the hydrophilic treatment is plasma treatment, and the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
Further, respectively adding deionized water into pulp fiber slurry and chopped fiber slurry to carry out fluffing pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%; the grain size ratio of the pulp fiber slurry is less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of; according to the pulp fiber slurry: 10-80 wt% of chopped fiber slurry: and mixing the pulp fiber slurry with an aqueous solution of the chopped fiber slurry according to the proportion of 10-90 wt%.
Further, the mass concentration of sizing is 0.001-0.05wt% in wet papermaking; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is lower than the melting point, the vehicle speed is 2-80 m/min, the line pressure is 0-40N/mm, and the preheating times are 1-5 times; the hot rolling temperature is within the melting point range, the hot rolling temperature of the polymer without melting point is 200-400 ℃, the vehicle speed is 2-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5.
The invention provides application of the pulp fiber, and the pulp fiber is applied to the fields of papermaking, wear-resistant fillers, insulating packaging, filtering industry and cement pulp.
The invention provides application of the special paper, which is applied to the fields of insulation packaging, honeycomb core material, printing packaging, building waterproofing, ground covering, medical sterilization packaging, composite material reinforcement, lithium battery diaphragm and the like.
The technical scheme provided by the embodiment of the invention has the beneficial effects that:
(1) Compared with the fiber produced by the prior art, the fiber prepared by flash spinning has high crystallinity, the crystallinity of the fiber is improved by at least 5 percent, the fiber is highly split and fibrillated after being cut and pulped, the high crystallinity can improve the strength and the thermal stability of the special paper, the fiber is highly split and thinned after being cut and pulped, an effective three-dimensional interpenetrating network structure can be formed in the special paper, the peeling strength of the special paper is improved, and particularly, the fiber diameter range prepared by flash spinning is 0.1-20 mu m, wherein 80 percent of the fiber diameter range is 5-10 mu m, the fiber in the range is subjected to subsequent pulping treatment, so that the prepared fiber is more in forking, single fiber forking is at least more than 5 and is in a bulk shape, and the fiber has higher toughness due to the high crystallinity, thus the three-dimensional interpenetrating network structure is presented in the special paper, the fiber is fully bonded with chopped fibers, and the bonding strength between the fiber and the special paper is improved; secondly, more than 50% of the pulp fibers prepared by the application have at least two branches on the length of 1mm, so that the tensile strength of the prepared special paper in all directions can be greatly improved, and the preparation probability of the special paper is improved. Compared with the special paper prepared by the prior art, the special paper prepared by the method can improve the peeling strength by more than 10 percent and the puncture resistance strength by more than 10 percent.
(2) The invention limits the grain size proportion of pulp fiber, the proportion of the grain size is not more than one third of the proportion of the pulp fiber which is larger than 10 meshes, the proportion of the pulp fiber which is smaller than or equal to 100 meshes is larger than 10%, the fiber with small grain size is less in bifurcation after pulping, but has higher degree of freedom, is easy to bend, has lower degree of freedom of the fiber with larger grain size, is more in bifurcation after pulping, and can lead the three-dimensional network structure to be uniformly distributed on the space structure of the product only by the mutual matching of the small grain size, the medium grain size and the large grain size, thus being difficult to cause agglomeration or segregation and having uniform mechanical property.
(3) The special paper is prepared by adopting the papermaking process, the chopped fibers can penetrate through the thickness of the whole paper sheet, the pulp fibers can be effectively overlapped with each other, and the long fibers penetrate through the thickness direction of the whole special paper, so that the problem of low peeling strength of the special paper is solved. In the pulping process, the structural uniformity of the special paper is effectively improved through means of pulping, surface treatment, dispersing agents and the like. In the papermaking process, the fine gaps are reserved in the paper sheet after the fibers are uniformly filtered, so that the air permeability and the moisture vapor transmission rate of the special paper are improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a polarized light micrograph of a polyethylene flash spun fiber prepared according to example 1 of the present invention;
FIG. 2 is a polarized light micrograph of a polyethylene pulp fiber prepared according to example 1 of the present invention;
fig. 3 is an SEM image of the polyethylene specialty paper prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and the embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent.
The embodiment of the invention discloses special paper, which comprises at least two types of fibers, wherein the pulp fibers comprise 10-80 wt% of pulp fibers relative to the total weight of the special paper, and the chopped fibers comprise 10-90 wt% of chopped fibers relative to the total weight of the special paper; the pulp fiber is prepared by flash spinning, more than 50% of the pulp fiber has at least two branches on the length of 1mm, the beating degree is 10-80 DEG SR after cutting, pulping and beating, the length of the chopped fiber is 3-10 mm, the fiber denier is 1-3D, and the special paper is prepared by wet papermaking, squeezing, drying and hot pressing treatment after mixing.
Compared with the fiber produced by the prior art, the fiber prepared by flash spinning has high crystallinity, the crystallinity of the fiber is improved by at least 5 percent, the fiber is highly split and finely fibrillated after being cut and pulped, the high crystallinity can improve the strength of special paper, the fiber is highly split and finely split after being cut and pulped, an effective three-dimensional interpenetrating network structure can be formed in the special paper, the peeling strength of the special paper is improved, and in particular, the fiber prepared by flash spinning has the diameter range of 0.1-18 mu m, wherein 80 percent of the fiber has the diameter range of 5-10 mu m, the fiber in the range is subjected to subsequent pulping treatment, so that the prepared fiber is more in bifurcation, single fiber bifurcation is at least more than 5 and is in a bulk shape, and the fiber has higher toughness due to the high crystallinity, so that the fiber presents a three-dimensional interpenetrating network structure in the special paper and is fully bonded with chopped fibers, and the bonding strength between the fiber and the special paper is improved; secondly, more than 50% of the pulp fibers prepared by the application have at least two branches on the length of 1mm, so that the tensile strength of the prepared special paper in all directions can be greatly improved, and the preparation probability of the special paper is improved. Compared with the special paper prepared by the prior art, the special paper prepared by the method can improve the peeling strength by more than 10 percent and the puncture resistance strength by more than 10 percent.
It should be noted that 50% or more of the pulp fibers have at least two branches over a length of 1mm, i.e., a plurality of pulp fibers are selected, and observed through a mirror, the number of branches is observed within a length dimension of 1mm, if the number of branches of the same pulp fiber exceeds two, the number is counted, and finally, the ratio of the counted number to the total pulp fiber number is calculated, and for accurate detection results, the invention makes observation statistics on at least 50 pulp fibers.
Specifically, the diameter range of pulp fiber is 0.1-18 mu m, wherein 80% of the diameter range is 5-10 mu m, the length after cutting is 0.1-20.0 mm, and the particle size ratio of pulp fiber is less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1. the diameter range of pulp fibers prepared by flash spinning is 0.1-18 mu m, in order to achieve better pulping and form an effective three-dimensional interpenetrating network structure in special paper, the short cutting length and the grain size ratio of the pulp fibers are limited, in particular, the length after cutting is 0.1-20 mm, the proper size length can ensure that the refined fibers after pulping can form an effective network structure in a product, the comprehensive mechanical properties of the product are improved, such as stripping strength and puncture resistance, the cutting length has a negative effect on pulp uniformity, the pulping uniformity is improved due to shorter length, and the comprehensive mechanical properties of the product are reduced; finally, the grain size ratio of pulp fibers is limited, the grain size ratio is not more than one third of the grain size ratio which is larger than 10 meshes and is smaller than or equal to 100 meshes, the grain size ratio is larger than 10%, the branching of the small grain size fibers after pulping is less, the degree of freedom is higher, the fibers are easy to bend, the degree of freedom of the large grain size fibers is lower, the branching of the large grain size fibers after pulping is more, the three-dimensional net structure can be uniformly distributed on the space structure of the product only by the mutual matching of the small grain size, the medium grain size and the large grain size, agglomeration or segregation is not easy to cause, and the mechanical property is uniform.
Specifically, the pulp fiber has a profile of 20% -80%. Compared with other technologies, the crystallinity of the pulp fiber prepared by flash spinning is improved by at least 5 percent, but the crystallinity is not more than 90 percent, the crystallinity is proper, the strength of the fiber is larger due to the overhigh crystallinity, and the mechanical properties of the prepared product in all directions are easy to be uneven; secondly, the amorphous pulp fiber is easier to produce wrapping property with other fibers, and the pulp fiber prepared by flash spinning can ensure the uniformity of mechanical properties and the bonding strength of the two fibers. The calculation formula of the dysmorphism adopts the existing calculation mode, namely: in general, the higher the degree of the special-shaped degree is, the better the mechanical properties such as tensile strength of the special paper are, but the higher the degree of the special-shaped degree is, the condition that part of fibers are entangled to generate ropes in the subsequent beating process cannot realize a better net structure, so the degree of the special-shaped degree is limited.
Specifically, the mass ratio of the pulp fiber to the chopped fiber is 1: (1.2 to 1.5). The chopped fibers can penetrate through the thickness of the paper sheet, the pulp fibers have more branches and are in three-dimensional lap joint with the chopped fibers, and the long fibers penetrate through the thickness direction of the whole special paper, so that when the chopped fibers and the pulp fibers are in the range, the optimal performance can be realized.
Specifically, the degree of irregularity of the chopped fibers is 30-80%. The chopped fiber mainly provides a skeleton effect, so that the mechanical property of the product is improved, and the higher the degree of special shape of the chopped fiber is, the higher the bonding strength of the chopped fiber and other fibers is.
The invention also provides a preparation method of the special paper, which comprises the following steps:
S1, preparing pulp fiber slurry.
Adding a polymer and a solvent R1 into a reaction kettle, controlling the temperature of the reaction kettle to be higher than an upper critical dissolution temperature for at least 1min, then reducing the temperature to be lower than the upper critical dissolution temperature for 1-600 s at a cooling rate of at least 5 ℃/min, increasing the temperature to be higher than the upper critical dissolution temperature for 6-600 s at a heating rate of at least 5 ℃/min, repeating the temperature reducing and heating processes, maintaining the pressure to be at least 3Mpa, and preparing the flash spinning fiber in a flash evaporation mode.
Or adding the polymer and the solvent R1 into a reaction kettle, controlling the pressure of the reaction kettle to be higher than the cloud point pressure for at least 1min, then reducing the pressure to be lower than the cloud point pressure for 60-2000 s at a reducing speed of at least 0.05MPa/min, increasing the pressure to be higher than the cloud point pressure for 60-2000 s at a increasing speed of at least 0.05MPa/min, repeating the reducing and increasing processes, maintaining the temperature to be higher than at least the upper critical dissolution temperature, and preparing the flash spinning fiber through a flash evaporation mode.
The repeated cooling and heating process can be performed for 0 times, namely the repeated cooling and heating process can be performed for a plurality of times after only one cooling and heating process. The prepared flash spinning fiber can be more branched and the performance is greatly improved by repeating the temperature reducing and rising processes for a plurality of times.
The precipitated fibers can be refined by adopting higher heating and cooling speeds based on the critical dissolution temperature. Specifically, after cooling, after separating out finer fibers, through heating up, dissolve partial fibers to form more fiber crystal nuclei, through repeated many times, the crystal nuclei quantity increases, in the follow-up flash spinning in-process, makes the pulp fiber of preparation more than 50% have two at least branches on 1 mm's length.
In the present invention, the "repeating the buck and boost process" may be 0 times, i.e., the buck and boost process may be repeated a plurality of times through only one buck and boost process. Through repeated depressurization and pressurization processes, the prepared flash spinning fiber can be more branched, and the performance is greatly improved.
By using higher pressure boosting and reducing rates based on cloud point pressure, the precipitated fibers can be refined. Specifically, after depressurization, after separating out finer fibers, part of the fibers are dissolved through pressure boosting, so that more fiber crystal nuclei are formed, the number of the crystal nuclei is increased through repeated repetition, and in the subsequent flash spinning process, more than 50% of the prepared pulp fibers have at least two branches on the length of 1 mm.
Since the use of the "upper critical solution temperature" has a similar effect to the "cloud point pressure", the present application is described in detail with reference to the upper critical solution temperature.
The polymer comprises polyolefin, polyester, polyether-ether-ketone and polyketone with melting points, and meta-aramid, para-aramid, polyarylate, poly-p-phenylene benzobisoxazole and polyimide without melting points; the solvent R1 is one or more of water, alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halogenated hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, aromatic hydrocarbon and unsaturated hydrocarbon.
The temperature and pressure in the reaction kettle are controlled by an auxiliary gas and a heating system cooling system, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
The flash evaporation mode is that polymer spinning solution is sprayed out into nitrogen with the temperature of 50-500 ℃ through a decompression spray head of flash evaporation spinning equipment; or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polymer through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70wt%.
It should be noted that the determination criteria adopted for the upper critical dissolution temperature, the cloud point pressure, the good solvent and the poor solvent are common knowledge in the art, and will not be described herein.
Cutting the flash spinning fiber to 0.1-20 mm, and pulping to obtain the pulp fiber with a beating degree of 10-80 DEG SR.
Cutting the flash spun fiber to 0.1-20 mm comprises: cutting off the flash spun fibers to obtain four kinds of length fibers with the length ranges of 0.1-0.4 mm, 2.5-3.5 mm, 9.5-10.5 mm and 18-20 mm respectively, and mixing the flash spun chopped fibers with the same mass and four kinds of length. The four lengths are respectively selected from the five ranges, and the physical lap joint between the fibers with different lengths is improved by limiting the lengths of the fibers, so that the prepared special paper has good peeling resistance.
The pulping treatment process comprises the following steps: adding deionized water to defibering for 5-50 min, wherein the slurry concentration during pulping is 0.01-0.1wt%, feeding a heavy cutter to defibering for 1-10 min, feeding a light cutter to defibering for 30-200 min.
It should be noted that the lower heavy knife is to increase specific pressure, adjust the gap between the fly knife roller (upper knife) and the bed knife to be 0.5-1.0mm, and cut the fiber strongly, so that the fiber has a fiber length suitable for papermaking by a paper machine; the lower light knife is to weaken specific pressure, adjust the clearance between a fly knife roller (upper knife) and a bottom knife to be 1.5-3.0mm, fully defiberize the fibers, fibrillate the fibers in the slurry as much as possible, and obtain the wet swelling and the fibrillation, so that the fiber has a fiber form suitable for papermaking by a paper machine. When the heavy knife is put down, the beating pressure is 10-20kg, and when the light knife is put down, the beating pressure is 1-5kg.
After pulping, the pulping degree of pulp fibers is 10-80 DEG SR, the pulping pressure of a heavy cutter is high and short, so that the fibers are expanded, the cohesion is reduced, the tissues in the fibers are relaxed, the contact area is effectively increased, the strength of the subsequent special paper is improved, the pulping time is not more than 10min, and the air permeability of the special paper is reduced after the large pulping pressure is used for a long time; the lower light knife has small beating pressure and long beating time, the fiber is split longitudinally, two ends are broomed, the fiber surface is split and fluffed, the specific surface area of the fiber is greatly increased, and the hydrogen chain combination is promoted.
And after drying, carrying out hydrophilic treatment on the pulp fiber to obtain the modified pulp.
S2, preparing chopped fiber slurry.
And carrying out hydrophilic treatment on the chopped fibers with the length of 3-10 mm, the fiber denier of 1-3D and the profile degree of 30-80%.
The chopped fibers used in the invention are cleaned by adopting a surfactant and deionized water before use to remove surface stains, and the surfactant can adopt ionic surfactants (including cationic surfactants, anionic surfactants and amphoteric surfactants), nonionic surfactants, compound surfactants, other surfactants and the like in the prior art. The surfactant adopted by the invention is sodium dodecyl benzene sulfonate.
S3, pulping the pulp fiber slurry and the chopped fiber slurry respectively, mixing the pulp and the chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
And respectively adding deionized water into the pulp fiber slurry and the chopped fiber slurry to carry out fluffing pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%. The grain size ratio of the pulp fiber slurry is less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1.
According to the pulp fiber slurry: 10-80 wt% of chopped fiber slurry: and mixing the pulp fiber slurry with an aqueous solution of the chopped fiber slurry according to the proportion of 10-90 wt%. The mass concentration of sizing is 0.001-0.05wt% in wet papermaking; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is lower than the melting point, the vehicle speed is 2-80 m/min, the line pressure is 0-40N/mm, and the preheating times are 1-5 times; the hot rolling temperature is within the melting point range, the hot rolling temperature of the polymer without melting point is 200-400 ℃, the vehicle speed is 2-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5.
For example, polyethylene has a melting point in the range of 85-136℃and a preheating temperature of less than 85℃and a hot rolling temperature of between 85-136 ℃. The para-aramid fiber has no melting point, and the hot rolling temperature is between 200 and 400 ℃.
The hot rolling process is realized by a hot roller, wherein the hot roller is a metal roller, a patterned roller or an elastic roller with patterns on the surface, and specific size parameters can be determined based on actual production conditions.
The hydrophilic treatment according to the application is to increase the surface energy of the fiber to at least 38mN/m. The surface of the fibers may be treated to increase the surface energy using prior art techniques. Corona treatment and plasma treatment are preferably used in the present application.
When the hydrophilic treatment is corona treatment, the corona treatment process comprises the following steps: the corona treatment voltage is 4000-16000V, the frequency is 12-26 KHz, the distance between the electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h.
When the hydrophilic treatment is plasma treatment, the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
The invention provides application of the pulp fiber, and the pulp fiber is applied to the fields of papermaking, wear-resistant filler, insulating packaging, filtering industry and cement slurry.
The invention provides application of the special paper, which is applied to the fields of insulation packaging, honeycomb core material, printing packaging, building waterproofing, ground covering, medical sterilization packaging, composite material reinforcement and lithium battery diaphragm.
In order to better illustrate the embodiments of the present invention, the present invention will be described in further detail by way of specific examples.
Example 1
The embodiment of the invention provides a preparation method of polyethylene special paper, which comprises the following steps of;
S1, preparing polyethylene pulp fiber slurry.
Preparation of polyethylene pulp fiber slurry: adding polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride into a reaction kettle, preserving heat for 1min at a temperature rising rate of 30 ℃/min to 200 ℃, reducing the temperature falling rate of 20 ℃/min to 140 ℃ and preserving heat for 5s, rising the temperature rising rate of 20 ℃/min to 200 ℃ and preserving heat for 6s, controlling the pressure in the kettle to 15MPa by nitrogen, obtaining spinning solution with the mass concentration of 10wt% of the polymer, and spraying the spinning solution through a decompression nozzle to obtain the flash-spun polyethylene fiber with the diameter range of 0.5-20um; the fiber strength was 3.5g/d, the crystallinity of the fiber was 65% and the profile was 20%, and the prepared polyethylene flash spun fiber was as shown in FIG. 1.
The performance index of the solitary petrochemical 5502XA is as follows: 2.16kg of raw material, the melt flow rate of which is measured to be 0.2g/10min by adopting ISO 1133; the density is 954kg/m 3 measured by ISO 1872/1; the tensile strength is 26MPa and the elongation at break is more than 300 percent by adopting ISO R527/2D.
Cutting off the polyethylene flash spinning fiber by using a cutter to obtain polyethylene flash spinning chopped fibers with lengths of 0.1mm, 3mm, 10mm and 20mm respectively, mixing the four lengths of the polyethylene flash spinning chopped fibers with the same weight, pulping simultaneously, adding deionized water to fluffe for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, and then feeding a heavy cutter to fluffe for 10min, feeding a light cutter to fluffe for 100min; filtering water, drying, carrying out corona treatment on the absolute dry polyethylene pulp fiber, wherein the voltage of the corona treatment is 4000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fiber is 8mm, and the air flow is 1000m 3/h; the resulting pulp fiber slurry had a pulp freeness of 48 ° SR, and the prepared pulp fiber was shown in fig. 2.
S2, preparing ultra-high molecular weight polyethylene chopped fiber slurry.
Cutting the ultra-high molecular weight polyethylene fiber with the cross section of broad bean shape and the degree of special-shaped 30% and fineness of 2D into 6mm, washing away the surface oil agent by adopting a sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, and carrying out oxygen plasma treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 300W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.02L/min.
S3, pulping the polyethylene pulp fiber slurry and the ultra-high molecular weight polyethylene chopped fiber slurry respectively, mixing the pulp and the ultra-high molecular weight polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 2:7:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.01 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of pulp fiber of 60wt% and the absolute dry weight of ultra-high molecular weight polyethylene chopped fiber of 40wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine is 0.001wt% during papermaking; obtained by squeezing and drying, the preheating temperature is 85 ℃, the vehicle speed is 2m/min, the line pressure is 40N/mm, and the preheating times are 2 times; the hot rolling temperature is 125 ℃, the speed is 2m/min, the line pressure is 100N/mm, the hot rolling is carried out for 2 times, the polyethylene special paper is obtained, the ration of the polyethylene special paper is 40g/m 2, the thickness is 115um, and the prepared polyethylene special paper is shown in figure 3.
Example 2
The embodiment of the invention provides a preparation method of polyethylene special paper, which comprises the following steps of;
S1, preparing polyethylene pulp fiber slurry.
Preparation of polyethylene pulp fiber slurry: adding polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride into a reaction kettle, preserving heat for 2min at a temperature rising rate of 5 ℃/min to 200 ℃, preserving heat for 1s at a temperature falling rate of 5 ℃/min to 140 ℃, rising the temperature at the temperature rising rate of 5 ℃/min to 200 ℃ and preserving heat for 6s, controlling the pressure in the kettle to reach 3MPa by nitrogen, obtaining spinning solution with the mass concentration of 10wt% of the polymer, and spraying the spinning solution through a decompression nozzle to obtain the flash-spun polyethylene fiber with the diameter range of 0.5-20um; the fiber strength was 3.5g/d, the crystallinity of the fiber was 63%, and the profile was 22%.
Cutting off the polyethylene flash spinning fiber by using a cutter to obtain polyethylene flash spinning chopped fibers with lengths of 0.2mm, 2.5mm, 9.5mm and 18mm respectively, mixing the four lengths of the polyethylene flash spinning chopped fibers with the same weight, pulping simultaneously, adding deionized water to defiberize for 50min, wherein the mass concentration of the slurry during pulping is 0.01wt%, feeding a heavy cutter to defiberize for 1min, feeding a light cutter to defiberize for 30min; filtering water, drying, and carrying out corona treatment on the absolute dry polyethylene pulp fiber, wherein the voltage of the corona treatment is 4000V, the frequency is 12KHz, the distance between an electrode rod and the absolute dry polymer fiber is 10mm, and the air flow is 300m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 11 DEG SR.
S2, preparing ultra-high molecular weight polyethylene chopped fiber slurry.
Cutting the ultra-high molecular weight polyethylene fiber with the cross section of broad bean shape and the degree of special-shaped 30% and fineness of 2D into 3mm, washing away the surface oil agent by adopting a sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, and carrying out oxygen plasma treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 200W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.008L/min.
S3, pulping the polyethylene pulp fiber slurry and the ultra-high molecular weight polyethylene chopped fiber slurry respectively, mixing the pulp and the ultra-high molecular weight polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 8:1:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.01 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of pulp fiber being 90wt%, and the absolute dry weight of ultra-high molecular weight polyethylene chopped fiber being 10wt%, wherein the sizing mass concentration of a paper machine is 0.001wt% when the paper machine is used for papermaking; obtained by squeezing and drying, the preheating temperature is 85 ℃, the vehicle speed is 2m/min, the line pressure is 0N/mm, and the preheating times are 2 times; the hot rolling temperature is 120 ℃, the speed is 2m/min, the line pressure is 100N/mm, the hot rolling times are 2 times, and the polyethylene special paper is obtained, the ration of the polyethylene special paper is 40g/m 2, and the thickness is 115um.
Example 3
The embodiment of the invention provides a preparation method of polyethylene special paper, which comprises the following steps of;
S1, preparing polyethylene pulp fiber slurry.
Preparation of polyethylene pulp fiber slurry: adding polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride into a reaction kettle, preserving heat for 1min at a heating rate of 10 ℃/min to 200 ℃, reducing the temperature to 140 ℃ at a cooling rate of 20 ℃/min, preserving heat for 600s, heating to 200 ℃ at a heating rate of 20 ℃/min, preserving heat for 600s, controlling the pressure in the kettle to reach 5MPa by nitrogen, obtaining spinning solution with the mass concentration of 10wt% of the polymer, and spraying the spinning solution through a decompression nozzle to obtain the flash-spun polyethylene fiber with the diameter range of 0.5-20um; the fiber strength is 3.5g/d, the crystallinity of the fiber is 60%, and the profile is 20%.
Cutting off the polyethylene flash spinning fiber by using a cutter to obtain polyethylene flash spinning chopped fibers with lengths of 0.4mm, 3.5mm, 10.5mm and 20mm respectively, mixing the four lengths of the polyethylene flash spinning chopped fibers with the same weight, pulping simultaneously, adding deionized water to defiberize for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, and then, feeding a heavy cutter to defiberize for 10min, feeding a light cutter to defiberize for 200min; filtering water, drying, and carrying out corona treatment on the absolute dry polyethylene pulp fiber, wherein the voltage of the corona treatment is 16000V, the frequency is 26KHz, the distance between an electrode rod and the absolute dry polymer fiber is 8mm, and the air flow is 6000m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 78 DEG SR.
S2, preparing ultra-high molecular weight polyethylene chopped fiber slurry.
Cutting the ultra-high molecular weight polyethylene fiber with the cross section of broad bean shape and the degree of special-shaped 30% and fineness of 2D into 10mm, washing away the surface oil agent by adopting a sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, and carrying out oxygen plasma treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 500W, the treatment time is 6min, and the volume flow of high-purity oxygen is 0.02L/min.
S3, pulping the polyethylene pulp fiber slurry and the ultra-high molecular weight polyethylene chopped fiber slurry respectively, mixing the pulp and the ultra-high molecular weight polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:8:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.1 wt%.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of pulp fiber of 30wt% and the absolute dry weight of ultra-high molecular weight polyethylene chopped fiber of 70wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine is 0.001wt% during papermaking; obtained by squeezing and drying, the preheating temperature is 85 ℃, the vehicle speed is 80m/min, the line pressure is 40N/mm, and the preheating times are 2 times; the hot rolling temperature is 125 ℃, the speed is 100m/min, the line pressure is 100N/mm, the hot rolling times are 2 times, and the polyethylene special paper is obtained, the ration of the polyethylene special paper is 40g/m 2, and the thickness is 115um.
Example 4
Unlike example 1, in the present example, in S3, the aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 46wt% and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 54 wt%.
Example 5
Unlike example 1, in the present example, in S3, the aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 40wt% and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 60 wt%.
Example 6
The embodiment of the invention provides a preparation method of polyester special paper, which comprises the following steps of;
S1, preparing a polyester pulp fiber slurry.
Preparation of a polyester pulp fiber slurry: adding polyester (instrumentation chemical fiber FC 510), normal hexane and chloroform into a reaction kettle (the mass ratio of the normal hexane to the chloroform is 1:2), preserving heat for 2min at a temperature rising rate of 30 ℃/min to 250 ℃, reducing the temperature falling rate of 20 ℃/min to 200 ℃, preserving heat for 60s at a temperature rising rate of 20 ℃/min to 250 ℃, preserving heat for 60s at a temperature reducing rate of 5 ℃/min to 220 ℃, preserving heat for 6s at a temperature rising rate of 10 ℃/min to 250 ℃, preserving heat for 10s at a temperature rising rate of 10 ℃/min, controlling the pressure in the kettle to be 14MPa by nitrogen, obtaining spinning solution with the mass concentration of 10wt% of polymer, and spraying the spinning solution through a pressure reducing nozzle to obtain polyester flash spinning fibers with the fiber diameter range of 0.1-20um; the fiber strength is 4.5g/d, the crystallinity of the fiber is 56%, and the profile is 20%.
Cutting the polyester flash spinning fiber by using a cutter to obtain polyester flash spinning chopped fibers with lengths of 0.1mm, 3mm, 10mm and 20mm respectively, mixing the polyester flash spinning chopped fibers with four lengths of the same weight, pulping at the same time, adding deionized water to fluffe for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, and then fluffing for 1min, and then fluffing for 30min by using a light cutter; filtering water, drying, carrying out corona treatment on the absolute dry short fibers, wherein the voltage of the corona treatment is 5000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fibers is 5mm, and the air flow is 1000m 3/h; the polyester pulp fiber slurry is obtained, and the pulp beating degree is 20 DEG SR.
S2, preparing polyester chopped fiber slurry.
Cutting polyester fiber with the special-shaped degree of 30% and the fineness of 1.9D into 6mm, washing away the surface oil agent by using sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, carrying out corona treatment on the absolute-dry polyester chopped fiber, wherein the voltage of the corona treatment is 14000V, the frequency is 20KHz, the distance between an electrode rod and the absolute-dry polymer fiber is 10mm, and the air flow rate is 600m 3/h.
S3, pulping the polyester pulp fiber slurry and the polyester chopped fiber slurry respectively, mixing the pulp and the polyester chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyester pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:8:1, mechanically dispersing the mixed polyester pulp fiber slurry and deionized water, and concentrating to obtain the aqueous solution of the polyester pulp fiber slurry with the mass concentration of 0.01 weight percent.
Mechanically defibering the polyester chopped fiber slurry, and concentrating to obtain an aqueous solution of the polyester chopped fiber slurry with the mass concentration of 0.01 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of polyester pulp fiber being 90wt% and the absolute dry weight of polyester chopped fiber being 10wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine is 0.001wt% during papermaking; obtained by squeezing and drying, the preheating temperature is 185 ℃, the vehicle speed is 10m/min, the line pressure is 30N/mm, and the preheating times are 2 times; the hot rolling temperature is 215 ℃, the speed is 10m/min, the line pressure is 100N/mm, the hot rolling times are 2 times, and the polyester special paper is obtained, the ration of the polyester special paper is 70g/m 2, and the thickness is 100um.
Example 7
The embodiment of the invention provides a preparation method of meta-aramid 1313 special paper, which comprises the following steps of;
S1, preparing meta-aramid 1313 pulp fiber slurry.
Preparation of meta-aramid 1313 pulp fiber slurry: adding meta-aramid 1313, N-2-methylacetamide, dichloroacetic acid and lithium chloride into a reaction kettle (the mass ratio of the N, N-2-methylacetamide to the dichloroacetic acid is 2:1, the addition amount of the lithium chloride is 0.5 percent of the weight of the polymer), preserving heat for 1min at a temperature rising rate of 30 ℃/min to 150 ℃, preserving heat for 10s at a temperature reducing rate of 20 ℃/min, preserving heat for 9s at a temperature rising rate of 20 ℃/min to 150 ℃, controlling the pressure in the kettle to 8MPa by nitrogen, obtaining spinning solution with the mass concentration of 20 percent of the polymer, spraying the spinning solution through a decompression spray nozzle, and introducing hot nitrogen at 300 ℃ into a coagulating bath composed of glycerin and N, N-2-methylacetamide, wherein the content of the N, N-2-methylacetamide is 50 percent, obtaining meta-aramid flash evaporation fiber in the coagulating bath, and the fiber diameter range is 0.1-20um; the fiber strength is 6.5g/d, the crystallinity of the fiber is 50%, and the profile is 50%.
Cutting off the meta-aramid flash spun fibers by using a cutter to obtain meta-aramid flash spun chopped fibers with lengths of 0.1mm, 3mm, 10mm and 20mm respectively, mixing the four meta-aramid flash spun chopped fibers with the same weight, pulping at the same time, adding deionized water to defiberize for 5min, wherein the mass concentration of the pulp during pulping is 0.01wt%, and then, the pulp is subjected to heavy cutter and defibering for 1min, and then, the light cutter and the defiberize for 30min; filtering water, drying, carrying out corona treatment on the absolute dry short fibers, wherein the voltage of the corona treatment is 4000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fibers is 1mm, and the air flow is 1000m 3/h; the meta-aramid 1313 pulp fiber pulp is obtained, and the pulp beating degree is 25 DEG SR.
S2, preparing meta-aramid 1313 chopped fiber slurry.
Cutting the meta-aramid 1313 fiber with the profile degree of 40% and the fineness of 2D into 8mm, cutting the meta-aramid fiber with the profile degree of 30% and the fineness of 1D into 3mm, mixing the two fibers according to the same mass, washing away the surface oil agent by using a sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, performing oxygen plasma treatment on the absolute-dry meta-aramid 1313 chopped fiber, wherein the oxygen plasma treatment sets the ionization power to 300W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.02L/min.
S3, pulping pulp fiber slurry and meta-aramid 1313 chopped fiber slurry respectively, mixing the pulp fiber slurry and the meta-aramid 1313 chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
Meta-aramid 1313 pulp fiber slurry with the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 5:5:1, mechanically dispersing the mixed pulp fiber pulp and deionized water, and concentrating to obtain pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering meta-aramid 1313 chopped fiber slurry, and concentrating to obtain a polyester chopped fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Mixing the aqueous solution of the sizing agent, wherein the absolute dry weight of the meta-aramid 1313 pulp fiber is 90wt%, the absolute dry weight of the meta-aramid 1313 chopped fiber is 10wt%, and the sizing mass concentration of a paper machine is 0.001wt% when the paper machine is used for manufacturing paper; obtained by squeezing and drying, the preheating temperature is 250 ℃, the vehicle speed is 20m/min, the line pressure is 150N/mm, and the preheating times are 2 times; the hot rolling temperature is 300 ℃, the speed is 10m/min, the line pressure is 200N/mm, the hot rolling is carried out for 2 times, and the meta-aramid 1313 special paper is obtained, the ration of the meta-aramid 1313 special paper is 41g/m 2, and the thickness is 50um.
Example 8
The embodiment of the invention provides a preparation method of polyether-ether-ketone special paper, which comprises the following steps of;
s1, preparing polyether-ether-ketone pulp fiber slurry.
Preparing polyether-ether-ketone fiber slurry: adding polyether-ether-ketone (VICOTE Victrex Plc) and dichloroacetic acid into a reaction kettle, preserving heat for 1min at a temperature rising rate of 30 ℃/min to 220 ℃, preserving heat for 7s at a temperature falling rate of 20 ℃/min to 180 ℃, preserving heat for 7s at a temperature rising rate of 20 ℃/min to 220 ℃, controlling the pressure in the kettle to 14MPa by nitrogen, obtaining spinning solution with the mass concentration of 10wt% of polymer, and spraying the spinning solution through a decompression nozzle to obtain polyether-ether-ketone flash spinning fiber with the diameter range of 0.1-20 mu m; the fiber strength is 5.5g/d, the crystallinity of the fiber is 30%, and the profile is 56%.
Cutting the polyether-ether-ketone flash-spun fibers by using a cutter to obtain polyether-ether-ketone flash-spun chopped fibers with lengths of 0.1mm, 5mm, 10mm and 15mm respectively, mixing the four polyether-ether-ketone flash-spun chopped fibers with the same weight, pulping simultaneously, adding deionized water to defiberize for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, feeding a heavy cutter to defiberize for 5min, feeding a light cutter to defiberize for 10min; the fiber is filtered by water and dried, the absolute dry short fiber is subjected to corona treatment, the voltage of the corona treatment is 16000V, the frequency is 18KHz, the distance between an electrode rod and the absolute dry polymer fiber is 3mm, the air flow is 3000m 3/h, and the polyether-ether-ketone pulp fiber pulp with the pulp beating degree of 45 DEG SR is obtained.
S2, preparing polyether-ether-ketone chopped fiber slurry.
Cutting polyether-ether-ketone fiber with the special-shaped degree of 60% and fineness of 2.2D into 6mm, washing away a surface oiling agent by adopting a sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, and carrying out oxygen plasma treatment on the absolute dry polyether-ether-ketone chopped fiber, wherein the ionization power is set to be 300W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.02L/min.
S3, pulping the polyether-ether-ketone pulp fiber slurry and the polyether-ether-ketone chopped fiber slurry respectively, mixing the pulp and the polyether-ether-ketone chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyether-ether-ketone pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 8:1:1, mechanically dispersing the mixed pulp fiber pulp and deionized water, and concentrating to obtain pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering the polyether-ether-ketone chopped fiber slurry, and concentrating to obtain an aqueous solution of the polyether-ether-ketone chopped fiber slurry with the mass concentration of 0.01 wt%.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of the polyether-ether-ketone pulp fiber of 90wt% and the absolute dry weight of the polyether-ether-ketone chopped fiber of 10wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine during papermaking is 0.001wt%; obtained by squeezing and drying, the preheating temperature is 120 ℃, the vehicle speed is 50m/min, the line pressure is 30N/mm, and the preheating times are 2 times; the hot rolling temperature is 200 ℃, the speed is 50m/min, the line pressure is 120N/mm, the hot rolling times are 2 times, and the special polyether-ether-ketone paper is obtained, the ration of the special polyether-ether-ketone paper is 36g/m 2, and the thickness is 40um.
Example 9
The embodiment of the invention provides a preparation method of polylactic acid special paper, which comprises the following steps of;
S1, preparing polylactic acid pulp fiber slurry.
Preparing polylactic acid fiber slurry: adding polylactic acid (Daibou PLLA) and hexafluoroisopropanol into a reaction kettle, preserving heat for 1min at a temperature rising rate of 5 ℃/min to 100 ℃, preserving heat for 5s at a temperature reducing rate of 5 ℃/min to 30 ℃, rising the temperature at the temperature rising rate of 5 ℃/min to 100 ℃ and preserving heat for 10s, controlling the pressure in the kettle to reach 10MPa by argon, obtaining spinning solution with the mass concentration of 30wt% of polymer, and spraying the spinning solution through a decompression nozzle to obtain polylactic acid flash spinning fiber with the diameter range of 0.1-20um; the fiber strength is 2.8g/d, the crystallinity of the fiber is 40%, and the profile is 50%.
The Dai gang PLLA of the invention is hydroxyl-terminated L-polylactic acid OH-PLLA-OH, crystalline polymer, off-white to pale yellow irregular particles or powder. Glass transition temperature: 60-65 ℃, melting point: 170-180 ℃. The drying weight loss (%) is less than or equal to 0.5, the burning residue (%) is less than or equal to 0.5, the total heavy metal content (ppm) is less than or equal to 10, the catalyst residue (ppm) is less than or equal to 200, and the monomer residue (%) is less than or equal to 1.
Cutting off the polylactic acid flash spinning fiber by using a cutter to obtain polylactic acid flash spinning chopped fibers with lengths of 0.1mm, 3mm, 10mm and 15mm respectively, mixing the polylactic acid flash spinning chopped fibers with four lengths of the same weight, pulping at the same time, adding deionized water to fluffe for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, and then feeding a heavy cutter to fluffe for 2min, feeding a light cutter to fluffe for 200min; the fiber is filtered by water and dried, the absolute dry short fiber is subjected to corona treatment, the voltage of the corona treatment is 6000V, the frequency is 12KHz, the distance between an electrode rod and the absolute dry polymer fiber is 5mm, the air flow is 6000m 3/h, and the polylactic acid pulp fiber pulp with the pulp beating degree of 38 DEG SR is obtained.
S2, preparing polylactic acid chopped fiber slurry.
Cutting the 2D polylactic acid fiber with the abnormal degree of 70 percent and the fineness of 5mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oil, filtering and drying, and carrying out oxygen plasma treatment on the absolute dry polylactic acid chopped fiber, wherein the oxygen plasma treatment sets the ionization power to be 200W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.008L/min.
S3, respectively pulping the polylactic acid pulp fiber slurry and the polylactic acid chopped fiber slurry, mixing the pulp and the polylactic acid pulp fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polylactic acid pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:1:1, mechanically dispersing the mixed pulp fiber pulp and deionized water, and concentrating to obtain pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Mechanically defibering the polylactic acid chopped fiber slurry, and concentrating to obtain a polyester chopped fiber slurry aqueous solution with the mass concentration of 0.01 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of pulp fiber being 50wt% and the absolute dry weight of polylactic acid chopped fiber being 50wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine during papermaking is 0.05wt%; obtained by squeezing and drying, the preheating temperature is 95 ℃, the vehicle speed is 60m/min, the line pressure is 40N/mm, and the preheating times are 2 times; the hot rolling temperature is 175 ℃, the speed is 60m/min, the line pressure is 80N/mm, the hot rolling times are 2 times, and the polylactic acid special paper is obtained, the ration of the polylactic acid special paper is 150g/m 2, and the thickness is 250um.
Example 10
The embodiment of the invention provides a preparation method of polyarylate special paper, which comprises the following steps of;
S1, preparing polyarylate pulp fiber slurry.
Preparation of polyarylate fiber slurry: keeping the temperature of polyarylate and N-methylpyrrolidone at a heating rate of 5 ℃/min to 180 ℃ for 1min, reducing the temperature of 6 ℃/min to 130 ℃ for 5s, keeping the temperature of 180 ℃ at a heating rate of 5 ℃/min for 6s, controlling the pressure in a kettle to reach 10MPa by argon, obtaining a spinning solution with the polymer mass concentration of 30wt%, and spraying the spinning solution through a decompression spray nozzle to obtain the polyarylate flash-spun fiber with the fiber diameter range of 0.1-20um; the fiber strength is 5.3g/d, the crystallinity of the fiber is 40%, and the profile is 60%.
The polyarylate fibers are prepared based on the method disclosed in document [Lu H R, Li D S, Zhang Y, et al. Design of low dielectric constant and high 58 transparent polyarylate containing spiral ring [J]. Polymer, 2021, 228: 123948.].
Cutting the polyarylate flash-spun fibers by using a cutter to obtain polyarylate flash-spun chopped fibers with lengths of 0.1mm, 3mm, 10mm and 20mm respectively, mixing the four polyarylate flash-spun chopped fibers with the same weight, pulping at the same time, adding deionized water to fluffe for 5min, wherein the mass concentration of the slurry during pulping is 0.01wt%, feeding a heavy cutter to fluffe for 2min, feeding a light cutter to fluffe for 200min; the fibers are filtered by water and dried, the absolute dry short fibers are subjected to corona treatment, the voltage of the corona treatment is 6000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fibers is 1mm, the air flow is 1000m 3/h, and the polyarylate pulp fiber pulp with the pulp beating degree of 25 DEG SR is obtained.
S2, preparing polyarylate chopped fiber slurry.
Cutting 2D polyarylate fiber with the abnormal degree of 45 percent and the fineness of 5mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oil, filtering and drying, carrying out oxygen plasma treatment on the absolute dry polyester chopped fiber, setting the ionization power of 300W for 1min, and setting the volume flow of high-purity oxygen to be 0.02L/min.
S3, pulping the polyarylate pulp fiber slurry and the polyarylate chopped fiber slurry respectively, mixing the pulp and the polyarylate pulp fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The polyarylate pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:8:1, mechanically dispersing the mixed polyarylate pulp fiber pulp and deionized water, and concentrating to obtain the polyarylate pulp fiber pulp aqueous solution with the mass concentration of 0.01 weight percent.
Mechanically fluffing the polyarylate chopped fiber slurry, and concentrating to obtain a polyarylate chopped fiber slurry aqueous solution with the mass concentration of 0.1 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of the polyarylate pulp fiber of 30wt percent and the absolute dry weight of the polyarylate chopped fiber of 70wt percent, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine during papermaking is 0.001wt percent; obtained by squeezing and drying, the preheating temperature is 200 ℃, the vehicle speed is 10m/min, the line pressure is 50N/mm, and the preheating times are 2 times; the hot rolling temperature is 225 ℃, the speed is 10m/min, the line pressure is 100N/mm, the hot rolling is carried out for 1 time, and the polyarylate special paper is obtained, the ration of the polyarylate special paper is 100g/m 2, and the thickness is 130um.
Example 11
The embodiment of the invention provides a preparation method of poly (p-phenylene benzobisoxazole) special paper, which comprises the following steps of;
S1, preparing the poly (p-phenylene benzobisoxazole) pulp fiber slurry.
Preparation of poly (p-phenylene benzobisoxazole) fiber slurry: adding poly-p-phenylene benzobisoxazole and methanesulfonic acid into a reaction kettle, preserving heat for 1min at a temperature rising rate of 5 ℃/min to 180 ℃, reducing the temperature to 130 ℃ at a temperature reducing rate of 5 ℃/min, preserving heat for 7s, increasing the temperature to 180 ℃ at a temperature rising rate of 5 ℃/min, preserving heat for 10s, controlling the pressure in the kettle to reach 10MPa by argon, obtaining spinning solution with the mass concentration of 30wt% of polymer, and spraying the spinning solution through a decompression nozzle to obtain the poly-p-phenylene benzobisoxazole flash spinning fiber with the diameter range of 0.1-20 mu m; the fiber strength was 6.3g/d and the degree of profile was 50%.
Cutting off the poly-p-phenylene benzobisoxazole flash spun fiber by using a cutter to obtain poly-p-phenylene benzobisoxazole flash spun chopped fibers with the lengths of 0.1mm, 3mm, 10mm and 20mm respectively, mixing the poly-p-phenylene benzobisoxazole flash spun chopped fibers with the same weight and four lengths, pulping simultaneously, adding deionized water to fluffe for 5 minutes, wherein the mass concentration of the pulp during pulping is 0.01 weight percent, and then carrying out fluffing for 2 minutes, and then carrying out fluffing for 200 minutes; filtering water, drying, carrying out corona treatment on the absolute dry short fibers, wherein the voltage of the corona treatment is 7000V, the frequency is 26KHz, the distance between an electrode rod and the absolute dry polymer fibers is 8mm, and the air flow is 1000m 3/h; the polyarylate pulp fiber slurry is obtained, and the pulp beating degree is 27 DEG SR.
S2, preparing the poly-p-phenylene benzobisoxazole chopped fiber slurry.
Cutting 2D poly-p-phenylene benzobisoxazole fiber with the abnormal degree of 60 percent into 5mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oiling agent, filtering and drying, carrying out oxygen plasma treatment on the absolute dry polyester chopped fiber, wherein the oxygen plasma treatment sets the ionization power to be 500W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.02L/min.
S3, pulping the poly-p-phenylene benzobisoxazole pulp fiber slurry and the poly-p-phenylene benzobisoxazole chopped fiber slurry respectively, mixing the pulp according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper.
The poly (p-phenylene benzobisoxazole) pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:5:1, mechanically dispersing the mixed pulp fiber pulp and deionized water, and concentrating to obtain pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Mechanically fluffing the poly (p-phenylene benzobisoxazole) chopped fiber slurry, and concentrating to obtain a poly (p-phenylene benzobisoxazole) chopped fiber slurry aqueous solution with the mass concentration of 0.1 weight percent.
Mixing the aqueous solution of the slurry with the absolute dry weight of the poly (p-phenylene benzobisoxazole) pulp fiber being 90wt% and the absolute dry weight of the poly (p-phenylene benzobisoxazole) chopped fiber being 10wt%, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine is 0.05wt% during papermaking; obtained by squeezing and drying, the preheating temperature is 200 ℃, the vehicle speed is 20m/min, the line pressure is 150N/mm, and the preheating times are 2 times; the hot rolling temperature is 280 ℃, the speed is 20m/min, the line pressure is 200N/mm, the hot rolling times are 1 time, and the special paper of the poly-p-phenylene benzobisoxazole is obtained, the ration of the special paper of the poly-p-phenylene benzobisoxazole is 200g/m 2, and the thickness is 280um.
Example 12
Unlike example 1, in S1 of this example, the "cloud point pressure" was used as the spinning solution.
Preparation of polyethylene pulp fiber slurry: adding polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride into a reaction kettle, controlling the pressure in the kettle to reach 13MPa through nitrogen, maintaining for 5min, reducing the pressure reducing rate to 6MPa for 300s at 0.1MPa/min, increasing the pressure to 12MPa for 60s at the pressure increasing rate of 0.05MPa/min, controlling the temperature in the kettle to reach 200 ℃ to obtain spinning solution with the polymer mass concentration of 10wt%, and spraying the spinning solution through a decompression nozzle to obtain the polyethylene flash-spun fiber with the fiber diameter range of 0.5-20 mu m; the fiber strength was 3.7g/d, the crystallinity of the fiber was 64%, and the profile was 20%.
Comparative example 1
Unlike example 1, in S1 of this comparative example, polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride were added into a reaction vessel, the temperature rise rate was increased to 200℃at 30℃per minute, the pressure in the vessel was controlled to 15MPa by nitrogen gas, and a spinning solution having a polymer mass concentration of 10% by weight was obtained, and the spinning solution was discharged through a pressure reducing nozzle, to obtain a polyethylene flash spun fiber.
Comparative example 2
Unlike example 1, in S1 of this comparative example, polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride were added into a reaction vessel, the temperature was kept at a temperature rising rate of 3 ℃/min to 200℃for 1min, the temperature was kept at a temperature lowering rate of 3 ℃/min to 140℃for 5S, the temperature was raised at a temperature rising rate of 3 ℃/min to 200℃for 6S, the pressure in the vessel was controlled to 15MPa by nitrogen, a spinning solution having a polymer mass concentration of 10% was obtained, and the spinning solution was discharged through a pressure-reducing nozzle, whereby a polyethylene flash spun fiber was obtained.
Comparative example 3
Unlike example 1, in S3 of this comparative example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 8wt% and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 92 wt%.
Comparative example 4
Unlike example 1, in S3 of this comparative example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 92wt% and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 8 wt%.
Comparative example 5
Unlike example 1, in S3 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 9:8:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 6
Unlike example 1, in S3 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 1:1:1.1, mixing, mechanically dispersing the mixed polyethylene pulp fiber pulp and deionized water, and concentrating to obtain the polyethylene pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 7
Unlike example 1, in S3 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 8:9:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 8
Unlike example 12, in S1 of this comparative example, polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride were added into a reaction vessel, the pressure in the vessel was controlled to 13MPa by nitrogen gas and maintained for 5 minutes, the pressure was reduced to 6MPa at a pressure reduction rate of 0.01MPa/min and maintained for 300 seconds, the pressure was increased to 12MPa at a pressure increase rate of 0.001 ℃/min and maintained for 60 seconds, the temperature in the vessel was controlled to 200℃to obtain a spinning solution having a polymer mass concentration of 10% by weight, and the spinning solution was discharged through a pressure reduction nozzle to obtain a flash spun fiber of polyethylene.
The properties of the specialty papers prepared in examples 1 to 12 and comparative examples 1 to 8 were tested, test criteria: after the special paper is subjected to constant temperature and humidity treatment, the quantitative measurement standard is GB/T451.2-2002; the thickness measurement standard is GB/T451.3-2002; the measurement standard of tensile strength and elongation is GB/T12914-2008; the tear strength measurement standard is GB/T455-2002; the burst measurement standard is ISO 2758 (01); gurley air permeability measurement standard TAPPI T460; hydrostatic pressure measurement standard DIN EN 20811 (1992); peel strength test standard FZ/T80007.1-2006; puncture resistance strength test standard ASTM D3420. The results obtained by the detection are shown in Table 1.
TABLE 1 physical Property measurement results
The properties of the polyethylene specialty papers prepared in comparative examples 1 and 2 show that the precipitated fibers can be refined and the properties of the prepared polyethylene specialty papers can be improved by adopting higher heating and cooling speeds based on the critical dissolution temperature.
The properties of the polyethylene specialty papers prepared in comparative examples 12 and 8 are improved by refining the precipitated fibers with higher boost and buck speeds based on cloud point pressure.
As is apparent from comparative examples 1 and 3, when the content of the polyethylene pulp fiber is small, the polyethylene pulp fiber is difficult to form a compact three-dimensional structure with the ultra-high molecular weight polyethylene chopped fiber, resulting in poor performance; as is clear from comparative examples 1 and 4, when there are more polyethylene pulp fibers, three-dimensional penetrability between fibers and lap strength can be improved, but the properties of the prepared polyethylene specialty paper are poor due to the low content of ultra-high molecular weight polyethylene chopped fibers.
As is clear from comparative example 1 and comparative examples 5,6 and 7, the grain size ratio of the polyethylene pulp fiber is limited, and the grain size ratio is not more than one third of the grain size ratio of the polyethylene pulp fiber which is larger than 10 mesh and is smaller than or equal to 100 mesh, the branching of the small grain size fiber after pulping is less, but the degree of freedom is higher, the fiber is easy to bend, the degree of freedom of the large grain size fiber is lower, the branching of the small grain size fiber after pulping is more, the three-dimensional network structure can be uniformly distributed on the space structure of the product only by matching the small grain size, the medium grain size and the large grain size, agglomeration or segregation are not easy to cause, and the mechanical property is uniform, so the polyethylene special paper prepared in example 1 is excellent compared with comparative examples 5 to 7.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (12)
1. The special paper is characterized by comprising at least two types of fibers, wherein the pulp fibers comprise 10-80 wt% of the total weight of the special paper, and the chopped fibers comprise 10-90 wt% of the total weight of the special paper;
The pulp fiber is prepared by adopting flash spinning, more than 50% of the pulp fiber is provided with at least two branches on the length of 1mm, the beating degree is 10-80 DEG SR after cutting, pulping and beating, the length of the chopped fiber is 3-10 mm, the fiber denier is 1-3D, the special paper is prepared by wet papermaking, squeezing, drying and hot pressing treatment after mixing, and the polymer for preparing the pulp fiber is: polyolefin or polyester with melting point, or polyarylate or poly-p-phenylene benzobisoxazole without melting point;
the diameter range of pulp fibers is 0.1-18 mu m, wherein 80% of the diameter range is 5-10 mu m, the length after cutting is 0.1-20.0 mm, and the particle size ratio of the pulp fibers is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of;
The pulp fiber has a profile degree of 20% -80% and a crystallinity of not more than 90%;
the degree of irregularity of the chopped fibers is 30-80%.
2. The specialty paper according to claim 1, wherein the mass ratio of pulp fibers to chopped fibers is 1: (1.2 to 1.5).
3. The method for preparing the special paper according to any one of claims 1 to 2, comprising the following steps:
preparing pulp fiber slurry;
preparing a chopped fiber slurry;
pulping pulp fiber slurry and chopped fiber slurry respectively, mixing the pulp fiber slurry and the chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the special paper;
the preparation of the pulp fiber slurry comprises:
adding a polymer and a solvent R1 into a reaction kettle, controlling the temperature of the reaction kettle to be higher than an upper critical dissolution temperature for at least 1min, then reducing the temperature to be lower than the upper critical dissolution temperature for 1-600 s at a cooling rate of at least 5 ℃/min, increasing the temperature to be higher than the upper critical dissolution temperature for 6-600 s at a heating rate of at least 5 ℃/min, repeating the temperature reducing and heating processes, maintaining the pressure to be at least 3Mpa, and preparing flash spinning fibers in a flash evaporation mode;
Or adding the polymer and the solvent R1 into a reaction kettle, controlling the pressure of the reaction kettle to be higher than the cloud point pressure for at least 1min, then reducing the pressure to be lower than the cloud point pressure for 60-2000 s at a reducing speed of at least 0.05MPa/min, increasing the pressure to be higher than the cloud point pressure for 60-2000 s at a increasing speed of at least 0.05MPa/min, repeating the reducing and increasing processes, maintaining the temperature to be higher than at least the upper critical dissolution temperature, and preparing the flash spinning fiber through a flash evaporation mode;
Cutting the flash spinning fiber to 0.1-20 mm, and pulping to obtain pulp fiber with a beating degree of 10-80 DEG SR;
After drying, carrying out hydrophilic treatment on the pulp fiber to obtain the pulp;
The preparation of the chopped fiber slurry includes:
And carrying out hydrophilic treatment on the chopped fibers with the length of 3-10 mm, the fiber denier of 1-3D and the profile degree of 30-80%.
4. The method for preparing the special paper according to claim 3, wherein the pulping treatment process is as follows: adding deionized water to defibering for 5-50 min, wherein the slurry concentration during pulping is 0.01-0.1wt%, feeding a heavy cutter to defibering for 1-10 min, feeding a light cutter to defibering for 30-200 min.
5. The method for preparing the special paper according to claim 3, wherein the solvent R1 is one or more of water, alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halogenated hydrocarbon, aliphatic hydrocarbon and aromatic hydrocarbon;
The temperature and pressure in the reaction kettle are controlled by an auxiliary gas and a heating system cooling system, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
6. The method for preparing the special paper according to claim 3, wherein the flash evaporation mode is that polymer spinning solution is sprayed into nitrogen with the temperature of 50-500 ℃ through a decompression nozzle of flash evaporation spinning equipment;
Or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polymer through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70wt%.
7. The method of producing specialty paper according to claim 3, wherein cutting the flash spun fiber to 0.1 to 20mm comprises: cutting off the flash spun fibers to obtain four kinds of length fibers with the length ranges of 0.1-0.4 mm, 2.5-3.5 mm, 9.5-10.5 mm and 18-20 mm respectively, and mixing the flash spun chopped fibers with the same mass and four kinds of length.
8. A method of making specialty paper according to claim 3, wherein the hydrophilization treatment is to raise the surface energy of the fibers to at least 38 mN/m.
9. The method for preparing the special paper according to claim 8, wherein the hydrophilic treatment is corona treatment, and the corona treatment process is as follows: the voltage of corona treatment is 4000-16000V, the frequency is 12-26 KHz, the distance between an electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h;
Or the hydrophilic treatment is plasma treatment, and the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
10. The method for preparing the special paper according to claim 3, wherein deionized water is added into pulp fiber slurry and chopped fiber slurry respectively for fluffing and pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%;
The grain size ratio of the pulp fiber slurry is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of;
According to the pulp fiber slurry: 10-80 wt% of chopped fiber slurry: and mixing the pulp fiber slurry with an aqueous solution of the chopped fiber slurry according to the proportion of 10-90 wt%.
11. The method for preparing the special paper according to claim 10, wherein the mass concentration of sizing in the wet papermaking is 0.001-0.05 wt%; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is lower than the melting point, the vehicle speed is 2-80 m/min, the line pressure is 0-40N/mm, and the preheating times are 1-5 times; the hot rolling temperature is within the melting point range, the hot rolling temperature of the polymer without melting point is 200-400 ℃, the vehicle speed is 2-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5.
12. The special paper according to any one of claims 1-2 or the special paper prepared by the preparation method according to any one of claims 3-11, wherein the special paper is applied to the fields of insulation packaging, honeycomb core material, printing packaging, building waterproofing, ground covering, medical sterilization packaging, composite material reinforcement and lithium battery diaphragm.
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| CN102864677A (en) * | 2012-09-27 | 2013-01-09 | 陕西科技大学 | Para-aramid paper and preparation method thereof |
| CN110373955A (en) * | 2019-08-02 | 2019-10-25 | 吉林大学 | Polyetheretherketonefiber fiber extrusion coating paper and preparation method thereof |
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| CN109457533B (en) * | 2018-10-10 | 2021-04-23 | 华南理工大学 | Preparation method of regenerated aramid composite paper |
| CN110499669A (en) * | 2019-08-28 | 2019-11-26 | 恩若杰纳米技术(上海)有限公司 | A kind of environment-protection fiber paper and preparation method thereof |
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