CN106087094A - A kind of high intensity, the preparation method of modulus poly (vinyl alcohol) fine count fiber - Google Patents
A kind of high intensity, the preparation method of modulus poly (vinyl alcohol) fine count fiber Download PDFInfo
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- CN106087094A CN106087094A CN201610693236.7A CN201610693236A CN106087094A CN 106087094 A CN106087094 A CN 106087094A CN 201610693236 A CN201610693236 A CN 201610693236A CN 106087094 A CN106087094 A CN 106087094A
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- 239000000835 fiber Substances 0.000 title claims abstract description 47
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000009987 spinning Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005345 coagulation Methods 0.000 claims abstract description 8
- 230000015271 coagulation Effects 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 35
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 32
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 32
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 32
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 230000008602 contraction Effects 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 16
- 235000011152 sodium sulphate Nutrition 0.000 claims description 16
- 230000001112 coagulating effect Effects 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000006386 neutralization reaction Methods 0.000 claims description 10
- 239000013530 defoamer Substances 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 239000001117 sulphuric acid Substances 0.000 claims description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 238000006136 alcoholysis reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000002166 wet spinning Methods 0.000 abstract description 4
- 238000009512 pharmaceutical packaging Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- 238000006396 nitration reaction Methods 0.000 description 4
- 101100493712 Caenorhabditis elegans bath-42 gene Proteins 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000003637 basic solution Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
A kind of high intensity of the present invention, the preparation method of modulus poly (vinyl alcohol) fine count fiber, use boracic gel wet spinning technology to produce, and prepares through spinning solution preparation, coagulation forming, damp and hot stretching, dryness finalization.Fine count fiber prepared by the present invention, hot strength >=12.5CN/dtex, elastic modelling quantity >=280CN/dtex, initial melting temperature >=105 DEG C, line density 0.56 1.10dtex, extension at break 5 8%.The specific surface area of this kind fiber is big, paper-making process only needs add on a small quantity paper just can be greatly improved into after interfibrous Hyarogen-bonding, become that paper power is big, filterability and flexibility improve, the wettest anti-intensity, fracture strength increase, in 95 DEG C of hot water, shrinkage factor can be controlled in less than 1.5%, can be widely applied to build cover layer paper using, drug packaging, card paper using and other special dimension.
Description
One, technical field
The present invention relates to the preparation method of a kind of vinal, specifically a kind of high intensity, the poly-second of high-modulus
The preparation method of enol fine count fiber.
Two, background technology
Polyvinyl alcohol (PVA) fiber is widely used in weaving, garment material, coagulation because of the physical and chemical performance of its uniqueness
The fields such as soil enhancing, papermaking, and the most nontoxic, can natural degradation.
The production method of polyvinyl alcohol includes melt spinning method and the big class of solution spinning two, the production being currently mainly used
Method is solution spinning, and solution spinning is divided into wet spinning and dry spinning two kinds, wherein the solvent of wet spinning
Can be water, it is also possible to be organic solvent, the water-soluble polyvinyl alcohol fibers that such as the Kuraray company of Japan produces, its stock solution
Solvent be exactly methanol, the production technology of the current high strength high modulus polyvinyl alcohol fiber of China mainly uses water as solvent.
The existing related invention patent of the manufacture method of industrial vinal:
Patent CN201110238175.2 just describes a kind of high intensity, high-modulus, high-melting-point PVA fiber and manufacturer thereof
Method, the method uses boracic gel wet spinning technology, prepares including PVA spinning solution, filters, deaeration, spinning and post processing
Etc. step, the vinal using this technique to produce possesses following performance: intensity >=13.5CN/dtex, modulus >=
320CN/dtex, first fusing point >=108 DEG C, line density 2dtex.This kind fiber can be used for high-end industrial circle, as cement products,
Concrete enhancing etc..
Patent CN201210144517.9 describes a kind of fine-denier or superfine-denier polyvinyl alcohol fiber and preparation method thereof, should
Method includes, the preparation of polyvinyl alcohol spin dope, spinning solution molding obtain the steps such as the post processing of as-spun fibre, as-spun fibre
Suddenly, the fine count fiber produced dimension line density at 0.16-1.00dtex, hot strength 5-8cN/dtex, extension at break 5-15%,
Fiber is softening point in water Rp value 110-125 DEG C after formolation.This kind fine count fiber can be applicable to garment material field.
Field of papermaking is also an important application direction of vinal, particularly in special field of papermaking, as
The field such as drug packaging, security paper using, invoice paper using require the line density of vinals reach fine-denier rank (in China,
Generally the fiber of 0.9-1.4dtex is become fine count fiber；0.55-1.1dtex is fine-denier fiber), and intensity and modulus are relatively
High.Above-mentioned several fiber product all can not meet this requirement.
Three, summary of the invention
It is desirable to provide a kind of high intensity, the preparation method of modulus poly (vinyl alcohol) fine count fiber, to prepare
High intensity, the polyvinyl alcohol fine count fiber of high-modulus, meet the requirement in different application field.
High intensity of the present invention, the preparation method of modulus poly (vinyl alcohol) fine count fiber, comprise the steps:
1, spinning solution preparation
By degree of polymerization 1700-2000, the polyvinyl alcohol resin 12-17 mass parts of alcoholysis degree >=99% and deionized water 83-
88 mass parts mixing, dissolve at 98-115 DEG C 4-6 hour and obtain poly-vinyl alcohol solution, are subsequently adding boric acid, carbolic acid and gather
Ethers defoamer, with sulphuric acid or vinegar acid for adjusting pH value to 4.2-4.6, then is filtered by the metallic filter that filtering accuracy is 9-11 μm
Rear standing and defoaming 4-8 hour, it is thus achieved that spinning solution；
The addition of boric acid is the 1-2wt% of poly-vinyl alcohol solution quality, and phenolic addition is poly-vinyl alcohol solution
The 0.01-0.02wt% of quality, the addition of polyethers defoamer is the 0.3-0.4wt% of poly-vinyl alcohol solution quality.
2, coagulation forming
Described spinning solution is carried out spray webbing, strand by the spinning head of aperture 0.065-0.09mm after dosing pump measures
Curing molding in coagulating bath；
Sulfur acid sodium 340-400g/L in described coagulating bath, zinc sulfate 10-12g/L, sodium hydroxide 25-40g/L, hydrogen peroxide
0.018-0.022g/L, sodium sulfite 0.4-0.5g/L.Temperature 40-45 DEG C of described coagulating bath.
3, damp and hot stretching
Tow after step 2 solidifies is carried out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize,
Damp and hot drawing-off bath drawing-off, water washing bath washing and oil bath oil；
Described neutralization bath is the mixed aqueous solution of sodium sulfate and sulphuric acid, and wherein sodium sulphate content 240-260g/L, sulphuric acid contains
Amount 30-35g/L；Described temperature 48-55 DEG C neutralizing bath；
Described damp and hot drawing-off bath is the mixed aqueous solution of sodium sulfate and sulphuric acid, wherein sodium sulphate content 360-400g/L, sulfur
Acid content 30-35g/L；Temperature 88-92 DEG C of described damp and hot drawing-off bath；
The temperature of described water washing bath is 40-44 DEG C；
The temperature of described oil bath is 32-38 DEG C.
4, dryness finalization
Tow after step 3 being processed is dried heat treatment, it is thus achieved that polyvinyl alcohol fine count fiber；
Described dryness finalization include successively one section be dried, two-stage drying, preheating section, extension, contraction section and cooling section；
One section of dry temperature is 50-60 DEG C, 190-210 second drying time；The temperature of two-stage drying is 80-95 DEG C, dry
Dry second time 210-230；The temperature of preheating section is 160-180 DEG C, 110-130 second preheating time；The temperature of extension is 210-
225 DEG C, the extension of time 38-48 second；The temperature of contraction section is 200-215 DEG C, the contraction time 30-60 second；The temperature of cooling section is
20-50 DEG C, 30-60 second cool time.
Hot strength >=the 12.5CN/dtex of the polyvinyl alcohol fine count fiber that the present invention prepares, elastic modelling quantity >=
280CN/dtex, initial melting temperature >=105 DEG C, line density 0.56-1.10dtex, extension at break 5-8%.
The specific surface area of the polyvinyl alcohol fine count fiber that the present invention prepares is big, only needs to add on a small quantity in paper-making process
Interfibrous Hyarogen-bonding after paper just can be greatly improved into, becomes that paper power is big, filterability and flexibility improve, the wettest
Anti-intensity, fracture strength increase, and in 95 DEG C of hot water, shrinkage factor can be controlled in less than 1.5%, can be widely applied to building and cover
Layer paper using, drug packaging, card paper using and other special dimension.
The high intensity produced through above-mentioned steps, modulus poly (vinyl alcohol) fine count fiber are according to market demand optionally
It is wound and cuts off.
Beneficial effects of the present invention is embodied in:
1, in polyethylene alcohol basic solution process for preparation, add carbolic acid and can improve as-spun fibre section morphology, fibre section
Close to circular, it is simple to the super drawing of fiber.The addition of polyethers defoamer can reduce stock solution surface tension of liquid, improves former
Loss of thick fluid bubble effect, gives tow with flatness simultaneously, improves tow dispersibility and yield rate.
2, in coagulating bath, add hydrogen peroxide and sodium sulfite removes cyanogen root in polyethylene alcohol basic solution, by metal ion network
Close, it is to avoid metal ion concentration, around spray webbing aperture, extends the spinning head replacement cycle, improves spinning head performance, improves former
Liquid spinnability, production stability is greatly improved.In coagulating bath, add appropriate zinc sulfate can slow down as-spun fibre cortex
Formed, to greatest extent it is dehydrated, beneficially the super drawing in post processing.
3, this production technology is in addition to can producing fine count fiber, also slightly modified just can produce coarse denier fiber, water soluble fiber
Deng multi items vinal.
4, use two-part seasoning during fiber drying, just can realize being dried of tow with fewer energy, reduce
The production cost of fiber, the saving energy.
Four, detailed description of the invention
Below by example, the present invention is specifically described.Be necessary it is pointed out here that, following instance is served only for right
The present invention is further described, it is impossible to be interpreted as limiting the scope of the invention, and the person skilled in the art in this field can
The present invention made some nonessential improvement and adjustment according to foregoing invention content.
Embodiment 1:
High intensity in the present embodiment, modulus poly (vinyl alcohol) fine count fiber preparation method as follows:
1, spinning solution preparation
The degree of polymerization 1700, polyvinyl alcohol resin 12 mass parts of alcoholysis degree >=99% and deionized water 88 mass parts are mixed
Close, dissolve at 101 DEG C 5 hours and obtain poly-vinyl alcohol solution, be subsequently adding boric acid 1wt%, carbolic acid 0.01wt% and polyethers
Class defoamer 0.3wt%, with vinegar acid for adjusting pH value to 4.2, then stands after being filtered by the metallic filter that filtering accuracy is 10 μm
Deaeration 5 hours, it is thus achieved that spinning solution；
2, coagulation forming
By the spinning head of aperture 0.065mm, described spinning solution is carried out spray webbing after dosing pump measures, and strand is solidifying
Gu curing molding in Yu；Sulfur acid sodium 340g/L in described coagulating bath, zinc sulfate 10g/L, sodium hydroxide 25g/L, hydrogen peroxide
0.018g/L, sodium sulfite 0.4g/L.The temperature of described coagulating bath 42 DEG C.
3, damp and hot stretching
Tow after step 2 solidifies is carried out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize,
Damp and hot drawing-off bath drawing-off, water washing bath washing and oil bath oil, and detailed process is as follows:
Tow after solidification is placed in the neutralization bath of sodium sulphate content 240g/L, sulfuric acid content 30g/L and neutralizes, neutralize bath
Temperature 48 DEG C；Tow after neutralization carries out damp and hot in the damp and hot drawing-off of sodium sulphate content 360g/L, sulfuric acid content 30g/L is bathed
Drawing-off, the temperature 88 DEG C of damp and hot drawing-off bath；Tow after damp and hot drawing-off is washed in the water of 40 DEG C；Tow after washing enters
Enter in the oil bath of 32 DEG C and oil.
4, dryness finalization
Tow after step 3 being processed is dried heat treatment, and described dryness finalization includes one section of dry, two-stage nitration successively
Be dried, preheating section, extension, contraction section and cooling section, detailed process is as follows:
One section of dry temperature is 60 DEG C, 195 seconds drying times；The temperature of two-stage drying is 85 DEG C, drying time 216
Second；The temperature of preheating section is 180 DEG C, 130 seconds preheating time；The temperature of extension is 225 DEG C, extension of time 48 seconds；Contraction section
Temperature be 210 DEG C, contraction time 35 seconds；The temperature of cooling section is 28 DEG C, 50 seconds cool times.
It is 12.68CN/dtex that the present embodiment prepares the draw line intensity of fiber, and elastic modelling quantity is 285CN/dtex, incipient melting
Temperature is 106 DEG C, and line density is 0.56dtex, and extension at break is 6.5%.
Embodiment 2:
High intensity in the present embodiment, modulus poly (vinyl alcohol) fine count fiber preparation method as follows:
1, spinning solution preparation
The degree of polymerization 2000, polyvinyl alcohol resin 17 mass parts of alcoholysis degree >=99% and deionized water 83 mass parts are mixed
Close, dissolve at 115 DEG C 6 hours and obtain poly-vinyl alcohol solution, be subsequently adding boric acid 2wt%, carbolic acid 0.02wt% and polyethers
Class defoamer 0.4wt%, with vinegar acid for adjusting pH value to 4.5, then stands after being filtered by the metallic filter that filtering accuracy is 10 μm
Deaeration 6 hours, it is thus achieved that spinning solution；
2, coagulation forming
By the spinning head of aperture 0.09mm, described spinning solution is carried out spray webbing after dosing pump measures, and strand is in solidification
Curing molding in bath；Sulfur acid sodium 380g/L in described coagulating bath, zinc sulfate 12g/L, sodium hydroxide 35g/L, hydrogen peroxide
0.022g/L, sodium sulfite 0.48g/L.The temperature of described coagulating bath 44 DEG C.
3, damp and hot stretching
Tow after step 2 solidifies is carried out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize,
Damp and hot drawing-off bath drawing-off, water washing bath washing and oil bath oil, and detailed process is as follows:
Tow after solidification is placed in the neutralization bath of sodium sulphate content 255g/L, sulfuric acid content 35g/L and neutralizes, neutralize bath
Temperature 50 C；Tow after neutralization carries out damp and hot in the damp and hot drawing-off of sodium sulphate content 390g/L, sulfuric acid content 35g/L is bathed
Drawing-off, the temperature 91 DEG C of damp and hot drawing-off bath；Tow after damp and hot drawing-off is washed in the water of 42 DEG C；Tow after washing enters
Enter in the oil bath of 35 DEG C and oil.
4, dryness finalization
Tow after step 3 being processed is dried heat treatment, and described dryness finalization includes one section of dry, two-stage nitration successively
Be dried, preheating section, extension, contraction section and cooling section, detailed process is as follows:
One section of dry temperature is 60 DEG C, 190 seconds drying times；The temperature of two-stage drying is 95 DEG C, drying time 210
Second；The temperature of preheating section is 180 DEG C, 128 seconds preheating time；The temperature of extension is 225 DEG C, extension of time 45 seconds；Contraction section
Temperature be 205 DEG C, contraction time 40 seconds；The temperature of cooling section is 32 DEG C, 40 seconds cool times.
It is 12.97CN/dtex that the present embodiment prepares the draw line intensity of fiber, and elastic modelling quantity is 295CN/dtex, incipient melting
Temperature is 109 DEG C, and line density is 1.1dtex, and extension at break is 6.8%.
Embodiment 3:
High intensity in the present embodiment, modulus poly (vinyl alcohol) fine count fiber preparation method as follows:
1, spinning solution preparation
The degree of polymerization 1785, polyvinyl alcohol resin 15 mass parts of alcoholysis degree >=99% and deionized water 85 mass parts are mixed
Close, at 105 DEG C dissolve 5.5 hours obtain poly-vinyl alcohol solution, be subsequently adding boric acid 1.2wt%, carbolic acid 0.01wt% and
Polyethers defoamer 0.33wt%, with sulfur acid for adjusting pH value to 4.5, then after being filtered by the metallic filter that filtering accuracy is 10 μm
Standing and defoaming 6.5 hours, it is thus achieved that spinning solution；
2, coagulation forming
By the spinning head of aperture 0.07mm, described spinning solution is carried out spray webbing after dosing pump measures, and strand is in solidification
Curing molding in bath；Sulfur acid sodium 350g/L in described coagulating bath, zinc sulfate 11g/L, sodium hydroxide 30g/L, hydrogen peroxide
0.02g/L, sodium sulfite 0.48g/L.The temperature of described coagulating bath 42 DEG C.
3, damp and hot stretching
Tow after step 2 solidifies is carried out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize,
Damp and hot drawing-off bath drawing-off, water washing bath washing and oil bath oil, and detailed process is as follows:
Tow after solidification is placed in the neutralization bath of sodium sulphate content 248g/L, sulfuric acid content 32g/L and neutralizes, neutralize bath
Temperature 49 DEG C；Tow after neutralization carries out damp and hot in the damp and hot drawing-off of sodium sulphate content 365g/L, sulfuric acid content 35g/L is bathed
Drawing-off, the temperature 90 DEG C of damp and hot drawing-off bath；Tow after damp and hot drawing-off is washed in the water of 44 DEG C；Tow after washing enters
Enter in the oil bath of 36 DEG C and oil.
4, dryness finalization
Tow after step 3 being processed is dried heat treatment, and described dryness finalization includes one section of dry, two-stage nitration successively
Be dried, preheating section, extension, contraction section and cooling section, detailed process is as follows:
One section of dry temperature is 58 DEG C, 205 seconds drying times；The temperature of two-stage drying is 91 DEG C, drying time 214
Second；The temperature of preheating section is 175 DEG C, 119 seconds preheating time；The temperature of extension is 219 DEG C, extension of time 39 seconds；Contraction section
Temperature be 200 DEG C, contraction time 40 seconds；The temperature of cooling section is 35 DEG C, 38 seconds cool times.
It is 12.87CN/dtex that the present embodiment prepares the draw line intensity of fiber, and elastic modelling quantity is 290CN/dtex, incipient melting
Temperature is 107.5 DEG C, and line density is 1.02dtex, and extension at break is 5.7%.
Embodiment 4:
High intensity in the present embodiment, modulus poly (vinyl alcohol) fine count fiber preparation method as follows:
1, spinning solution preparation
The degree of polymerization 1850, polyvinyl alcohol resin 16 mass parts of alcoholysis degree >=99% and deionized water 84 mass parts are mixed
Close, dissolve at 104 DEG C 6 hours and obtain poly-vinyl alcohol solution, be subsequently adding boric acid 1.4wt%, carbolic acid 0.015wt% and gather
Ethers defoamer 0.36wt%, with vinegar acid for adjusting pH value to 4.5 more quiet after being filtered by the metallic filter that filtering accuracy is 10 μm
Put deaeration 7 hours, it is thus achieved that spinning solution；
2, coagulation forming
By the spinning head of aperture 0.08mm, described spinning solution is carried out spray webbing after dosing pump measures, and strand is in solidification
Curing molding in bath；Sulfur acid sodium 345g/L in described coagulating bath, zinc sulfate 10g/L, sodium hydroxide 25g/L, hydrogen peroxide
0.02g/L, sodium sulfite 0.45g/L.The temperature of described coagulating bath 42 DEG C.
3, damp and hot stretching
Tow after step 2 solidifies is carried out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize,
Damp and hot drawing-off bath drawing-off, water washing bath washing and oil bath oil, and detailed process is as follows:
Tow after solidification is placed in the neutralization bath of sodium sulphate content 245g/L, sulfuric acid content 35g/L and neutralizes, neutralize bath
Temperature 50 C；Tow after neutralization carries out damp and hot in the damp and hot drawing-off of sodium sulphate content 360g/L, sulfuric acid content 30g/L is bathed
Drawing-off, the temperature 92 DEG C of damp and hot drawing-off bath；Tow after damp and hot drawing-off is washed in the water of 44 DEG C；Tow after washing enters
Enter in the oil bath of 38 DEG C and oil.
4, dryness finalization
Tow after step 3 being processed is dried heat treatment, and described dryness finalization includes one section of dry, two-stage nitration successively
Be dried, preheating section, extension, contraction section and cooling section, detailed process is as follows:
One section of dry temperature is 58 DEG C, 205 seconds drying times；The temperature of two-stage drying is 90 DEG C, drying time 225
Second；The temperature of preheating section is 175 DEG C, 125 seconds preheating time；The temperature of extension is 220 DEG C, extension of time 42 seconds；Contraction section
Temperature be 205 DEG C, contraction time 55 seconds；The temperature of cooling section is 35 DEG C, 50 seconds cool times.
It is 12.95CN/dtex that the present embodiment prepares the draw line intensity of fiber, and elastic modelling quantity is 290CN/dtex, incipient melting
Temperature is 107 DEG C, and line density is 0.98dtex, and extension at break is 6.8%.
Claims (6)
1. a high intensity, the preparation method of modulus poly (vinyl alcohol) fine count fiber, it is characterised in that comprise the steps:
(1) spinning solution preparation
By degree of polymerization 1700-2000, the polyvinyl alcohol resin 12-17 mass parts of alcoholysis degree >=99% and deionized water 83-88 matter
Amount part mixing, dissolves at 98-115 DEG C 4-6 hour and obtains poly-vinyl alcohol solution, be subsequently adding boric acid, carbolic acid and polyethers
Defoamer, regulation pH value is to 4.2-4.6, then standing and defoaming 4-8 hour after being filtered by metallic filter, it is thus achieved that spinning solution；
(2) coagulation forming
By the spinning head of aperture 0.065-0.09mm, described spinning solution is carried out spray webbing after dosing pump measures, and strand is solidifying
Gu curing molding in Yu；
(3) damp and hot stretching
By through step (2) solidify after tow carry out damp and hot stretch processing, described damp and hot stretching successively include neutralize bath neutralize, wet
Hot gas spring bath drawing-off, water washing bath washing and oil bath oil；
(4) dryness finalization
Tow after step (3) being processed is dried heat treatment, it is thus achieved that polyvinyl alcohol fine count fiber；Described dryness finalization depends on
Secondary include one section be dried, two-stage drying, preheating section, extension, contraction section and cooling section.
Preparation method the most according to claim 1, it is characterised in that:
The addition of boric acid is the 1-2wt% of poly-vinyl alcohol solution quality, and phenolic addition is poly-vinyl alcohol solution quality
0.01-0.02wt%, the addition of polyethers defoamer is the 0.3-0.4wt% of poly-vinyl alcohol solution quality.
Preparation method the most according to claim 1, it is characterised in that:
The filtering accuracy of metallic filter is 9-11 μm.
Preparation method the most according to claim 1, it is characterised in that:
Sulfur acid sodium 340-400g/L in described coagulating bath, zinc sulfate 10-12g/L, sodium hydroxide 25-40g/L, hydrogen peroxide
0.018-0.022g/L, sodium sulfite 0.4-0.5g/L；Temperature 40-45 DEG C of described coagulating bath.
Preparation method the most according to claim 1, it is characterised in that:
Described neutralization bath is the mixed aqueous solution of sodium sulfate and sulphuric acid, wherein sodium sulphate content 240-260g/L, sulfuric acid content 30-
35g/L；Described temperature 48-55 DEG C neutralizing bath；
Described damp and hot drawing-off bath is the mixed aqueous solution of sodium sulfate and sulphuric acid, and wherein sodium sulphate content 360-400g/L, sulphuric acid contains
Amount 30-35g/L；Temperature 88-92 DEG C of described damp and hot drawing-off bath；
The temperature of described water washing bath is 40-44 DEG C；
The temperature of described oil bath is 32-38 DEG C.
Preparation method the most according to claim 1, it is characterised in that:
One section of dry temperature is 50-60 DEG C, 190-210 second drying time；The temperature of two-stage drying is 80-95 DEG C, when being dried
Between the 210-230 second；The temperature of preheating section is 160-180 DEG C, 110-130 second preheating time；The temperature of extension is 210-225
DEG C, the extension of time 38-48 second；The temperature of contraction section is 200-215 DEG C, the contraction time 30-60 second；The temperature of cooling section is 20-
50 DEG C, 30-60 second cool time.
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| CN108744039A (en) * | 2018-05-08 | 2018-11-06 | 佛山市第五人民医院（佛山市干部疗养院、佛山市工伤康复中心） | A kind of compound rest and preparation method thereof for organizational project anterior cruciate ligament |
| CN108948666A (en) * | 2018-07-06 | 2018-12-07 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of Automatic-inflating tyre repair liquid |
| CN110616503A (en) * | 2019-09-20 | 2019-12-27 | 陕西科技大学 | Polyvinyl alcohol spinning-based pressed paper and preparation method thereof |
| CN111101218A (en) * | 2018-10-26 | 2020-05-05 | 中国石油化工股份有限公司 | High-strength polyvinyl alcohol fiber for yarn and preparation method and application thereof |
| CN111778580A (en) * | 2020-07-08 | 2020-10-16 | 安徽皖维高新材料股份有限公司 | Concrete applicable polyvinyl alcohol fiber and preparation method thereof |
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| CN110616503B (en) * | 2019-09-20 | 2021-02-26 | 陕西科技大学 | Polyvinyl alcohol spinning-based pressed paper and preparation method thereof |
| CN111778580A (en) * | 2020-07-08 | 2020-10-16 | 安徽皖维高新材料股份有限公司 | Concrete applicable polyvinyl alcohol fiber and preparation method thereof |
| CN112226840A (en) * | 2020-08-04 | 2021-01-15 | 东华大学 | High-strength high-modulus PVA fiber and preparation method thereof |
| CN112226840B (en) * | 2020-08-04 | 2021-07-23 | 东华大学 | High-strength high-modulus PVA fiber and preparation method thereof |
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