CN113062004A - Method for preparing polyvinyl alcohol fiber by semi-molten wet method - Google Patents
Method for preparing polyvinyl alcohol fiber by semi-molten wet method Download PDFInfo
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- CN113062004A CN113062004A CN202110523616.7A CN202110523616A CN113062004A CN 113062004 A CN113062004 A CN 113062004A CN 202110523616 A CN202110523616 A CN 202110523616A CN 113062004 A CN113062004 A CN 113062004A
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 84
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 63
- 239000000835 fiber Substances 0.000 title claims abstract description 52
- 238000009987 spinning Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000004014 plasticizer Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 15
- 230000006835 compression Effects 0.000 claims abstract description 10
- 238000007906 compression Methods 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 238000007664 blowing Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000000265 homogenisation Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000009826 distribution Methods 0.000 claims abstract description 4
- 230000035611 feeding Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004804 winding Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006136 alcoholysis reaction Methods 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 238000000071 blow moulding Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000002166 wet spinning Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002074 melt spinning Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- -1 alcohol compound Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 229920002978 Vinylon Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
Images
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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
-
- 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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a method for preparing polyvinyl alcohol fiber by a semi-melting wet method, which comprises the steps of blending fiber-forming high polymer PVA resin and an environment-friendly plasticizer according to a certain mass ratio for plasticization, continuously feeding the mixture to a double-screw extruder through a screw feeder, and completing the processes of feeding, compression, melting, homogenization and the like of the PVA resin through the temperature distribution of each area of a screw; and filtering the completely molten PVA slurry, metering and pressurizing the completely molten PVA slurry by using a metering pump to a spinning assembly for spinning, and forming the nascent fiber by circular air blowing, and sequentially carrying out the process flows of multistage drying, hot stretching, oiling, coiling and the like to finally prepare the PVA fiber with the titer range of 100-400 dtex. The method can produce PVA fiber which can not be produced by the conventional wet process, and the titer of the PVA fiber is more than 20 dtex; in particular to special PVA fiber with the fineness of 100-400 dtex for the concrete industry, which meets the market demand.
Description
Technical Field
The invention relates to the technical field of PVA fiber preparation, in particular to a method for preparing polyvinyl alcohol fibers by a semi-molten wet method.
Background
The chemical fiber manufacturing process mainly comprises two major processes of melt spinning and wet spinning. The appearance of the fiber-forming polymer polyvinyl alcohol (PVA) is gradually changed when the fiber-forming polymer polyvinyl alcohol is heated to about 100 ℃. Partially alcoholyzed PVA began to melt at about 190 ℃ and decomposed at 200 ℃. The PVA with complete alcoholysis decomposes at about 210 ℃ and only starts to melt at about 220-230 ℃. Due to the special property of the thermal property of PVA, the material is not suitable for adopting the conventional melt spinning technical route. Vinylon (PVA fiber) spinning is the most typical wet spinning, PVA high polymer is used as a raw material, water is used as a solvent, and a PVA aqueous solution with a certain concentration is prepared; and (3) preparing the chemical fiber by adopting a wet spinning process. The process flow comprises the steps of spinning stock solution preparation (PVA dissolution), filtration, defoaming, pressure regulation, spinning (coagulating bath coagulation forming), heat treatment, winding (semi-finished product), cutting (short fiber) and after-finishing. The process flow is characterized in that:
1. the process flow is long, and the occupied area is large;
2. the water consumption is large, the salt content of the discharged sewage is high (Na2SO4), and the COD is high (low molecular PVA, NaAC and the like);
3. the steam consumption is high;
4. the necessary acid and base consumption;
5. the equipment needs a lot of special materials and a lot of process pipelines;
6. the fineness of the produced fiber is limited, and the general fineness range is 1-10 dtex;
7. the field operation environment is poor, and the number of operators is large. Particularly, the wet process can not produce special PVA fiber with the titer more than 20dtex, and restricts the widening of the application field of the fiber.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for preparing the polyvinyl alcohol fiber by the semi-melting wet method, which has the advantages of large fiber production range, no waste water discharge, good production environment, energy conservation and environmental protection.
The invention is realized by the following modes:
a method for preparing polyvinyl alcohol fiber by a semi-molten wet method comprises the following process steps:
s1: blending and plasticizing fiber-forming high polymer PVA resin and an environment-friendly plasticizer according to a certain proportion to obtain plasticized PVA resin;
s2: continuously feeding the plasticized PVA resin to a double-screw extruder through a screw feeder, and completing feeding, compression, melting and homogenizing metering of the plasticized PVA resin through temperature distribution of each area of the double-screw extruder to form molten PVA slurry; filtering the PVA slurry, metering and pressurizing by a metering pump to a spinning assembly, and spinning to obtain nascent fiber;
s3: and finally, preparing the PVA fiber with the titer of 3-600 dtex by the primary fiber through circular air blow molding, multistage drying, hot stretching, oiling and winding.
Further, the parameters of each process in the step S2 are set as:
setting the temperature of the double-screw extruder, wherein the feeding area is 105-115 ℃; a compression zone is 115-120 ℃; a melting zone is 125-130 ℃; the homogenization metering area is 130-135 ℃; spinning components are 100-120 ℃;
the diameter of a micropore of a spinning nozzle in the spinning assembly is 0.5-1.25, the length-diameter ratio is 1: 1-3: 1, and the drawing ratio of the spinning nozzle is 0.5-2 times;
further, the parameters of each process in the step S3 are set as:
circularly blowing air at the temperature of 20-40 ℃ and the air speed of 1-3 m/min;
the multistage drying and hot stretching temperature is 50-80 ℃ in a first section of oven; the rear section drying oven is increased according to the temperature gradient of 20-30 ℃; a preheating machine oven is 150-180 ℃; 190-210 ℃ of an stretcher oven; 170-200 ℃ of a shrinker oven;
the multistage drying and hot stretching speed is 0.5-2 times of the first section of oven speed; controlling the passing of tension by the remaining drying ovens, and increasing the speed of the latter section by 0.2-0.5 m/min compared with the speed of the former section; the hot stretching speed is 6-8 times of the speed of the first section of the drying oven; the cooling winding speed is 95-98% of the hot stretching speed;
the surface temperature of the wound fiber after cooling is not higher than 50 ℃.
Further, the polymerization degree of the PVA resin formed by the fiber-forming high polymer in the step S1 is 1700-2600, the alcoholysis degree is 98-99.8 mol%, and the coloration degree is more than or equal to 90%.
Further, the polymerization degree of the plasticized PVA resin in the step S1 is 1700-1800.
Further, the environment-friendly plasticizer is desalted water or alcohol compounds.
Further, the environment-friendly plasticizer accounts for 30-50% of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
Further, the environment-friendly plasticizer accounts for 42.5 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
Further, the environment-friendly plasticizer accounts for 43.2 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
Further, in the S3, the PVA fiber with the fineness of 100-400 dtex is finally prepared.
The invention has the beneficial effects that:
1. the invention thoroughly changes the situation that the PVA resin can only produce PVA fiber by a wet spinning technology, and adopts a new process similar to the melt spinning technology to produce the PVA fiber, thoroughly overcomes the defects of the wet spinning technology, and is a great breakthrough in the PVA fiber production technology.
2. The size range of the PVA fiber produced by the method is 3-600 dtex, and the more exact size range is 100-400 dtex.
3. Compared with the existing wet process, the semi-molten wet PVA fiber production method has the following advantages: a. the equipment arrangement is compact, and the occupied area is small; b. no wastewater discharge; c. no steam is needed (steam or heat transfer oil can be used for PVA plasticizing); d. no consumption of acid, alkali and mirabilite; e. the equipment material is mainly 304 stainless steel and A3F carbon steel, and the process pipelines are few; f. the field operation environment is good, and the number of required operators is small.
4. The double-screw extruder and the drying oven have simple structures and stable temperature and speed control.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a process flow diagram of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "provided," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example (b):
as shown in fig. 1, a method for preparing polyvinyl alcohol fiber by a semi-molten wet method comprises the following process steps:
s1: blending and plasticizing fiber-forming high polymer PVA resin and an environment-friendly plasticizer according to a certain proportion to obtain plasticized PVA resin;
s2: continuously feeding the plasticized PVA resin to a double-screw extruder through a screw feeder, and completing feeding, compression, melting and homogenizing metering of the plasticized PVA resin through temperature distribution of each area of the double-screw extruder to form molten PVA slurry; filtering the PVA slurry, metering and pressurizing by a metering pump to a spinning assembly, and spinning to obtain nascent fiber;
s3: and finally, preparing the PVA fiber with the titer of 3-600 dtex by the primary fiber through circular air blow molding, multistage drying, hot stretching, oiling and winding.
The parameters of each technological process in the steps are as follows:
setting the temperature of the double-screw extruder, wherein the feeding area is 105-115 ℃; a compression zone is 115-120 ℃; a melting zone is 125-130 ℃; the homogenization metering area is 130-135 ℃; spinning components are 100-120 ℃;
the diameter of a micropore of a spinning nozzle in the spinning assembly is 0.5-1.25, the length-diameter ratio is 1: 1-3: 1, and the drawing ratio of the spinning nozzle is 0.5-2 times;
circularly blowing air at the temperature of 20-40 ℃ and the air speed of 1-3 m/min;
the multistage drying and hot stretching temperature is 50-80 ℃ in a first section of oven; the rear section drying oven is increased according to the temperature gradient of 20-30 ℃; a preheating machine oven is 150-180 ℃; 190-210 ℃ of an stretcher oven; 170-200 ℃ of a shrinker oven;
the multistage drying and hot stretching speed is 0.5-2 times of the first section of oven speed; controlling the passing of tension by the remaining drying ovens, and increasing the speed of the latter section by 0.2-0.5 m/min compared with the speed of the former section; the hot stretching speed is 6-8 times of the speed of the first section of the drying oven; the cooling winding speed is 95-98% of the hot stretching speed;
the surface temperature of the wound fiber after cooling is not higher than 50 ℃.
In the step S1, the polymerization degree of the PVA resin is 1700-2600, the alcoholysis degree is 98-99.8 mol%, and the coloration degree is not less than 90%.
The polymerization degree of the plasticized PVA resin in the step S1 is 1700-1800.
The environment-friendly plasticizer is desalted water or alcohol compounds.
The environment-friendly plasticizer accounts for 30-50% of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
The environment-friendly plasticizer accounts for 42.5 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
The environment-friendly plasticizer accounts for 43.2 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
Further, in the S3, the PVA fiber with the fineness of 100-400 dtex is finally prepared.
Example 1:
raw materials: plasticizing PVA resin, wherein the polymerization degree is 1730, and the mass ratio of the plasticizer is 43.2%; melting: the temperature feeding area of the twin-screw extruder is 105 ℃; a compression zone of 115 ℃; a melting zone of 125 ℃; a homogenization and metering zone of 130 ℃; the spinneret pack was 105 ℃.
Spinning: the diameter of the micro-hole of the spinning nozzle is 0.6, the length-diameter ratio is 3:1, and the drawing ratio of the spinning nozzle is 2.05 times. Circular blowing is carried out at the temperature of 28 ℃ and the wind speed of 1.2 m/min. Multistage drying, hot stretching temperature: a first section of oven 55 ℃; the temperature of the second section of the oven is 80 ℃; the temperature of the third section of the oven is 95 ℃; the fourth section of the oven is at 120 ℃; preheating an oven 165 ℃; an extension oven is 195 ℃; shrink oven 175 ℃. Multistage drying and hot stretching speed: the first section of the oven speed is 7.0 m/min; the second section of the oven speed is 7.65 m/min; the speed of the third section of the oven is 7.8 m/min; the fourth section of the oven speed is 7.95 m/min; the speed of the preheating oven is 8.1 m/min; the speed of the extension oven is 70.0 m/min; shrink oven speed 69.6 m/min.
In example 1, the main control and technical quality indexes of the PVA fiber are as follows:
example 2:
raw materials: plasticizing PVA resin, wherein the polymerization degree is 1750, and the mass ratio of the plasticizer is 42.5%; melting: the temperature feeding area of the twin-screw extruder is 110 ℃; a compression zone of 120 ℃; a melting zone of 125 ℃; a homogenization and metering zone of 130 ℃; the spinneret assembly was 108 ℃.
Spinning: the diameter of the micro-hole of the spinneret is 0.8, the length-diameter ratio is 3:1, and the drawing ratio of the spinneret is 1.25 times. Circular blowing is carried out at the temperature of 30 ℃ and the wind speed of 1.5 m/min. Multistage drying, hot stretching temperature: a first section of oven 70 ℃; the temperature of the second section of the oven is 90 ℃; the temperature of a third section of the oven is 110 ℃; the fourth section of the oven is at 120 ℃; preheating an oven at 170 ℃; an extension oven is 195 ℃; the oven was shrunk 180 ℃. Multistage drying and hot stretching speed: the first section of the oven speed is 5.0 m/min; the second section of the oven speed is 5.2 m/min; the third section of the oven speed is 5.4 m/min; the fourth section of the oven speed is 5.6 m/min; the speed of the preheating oven is 5.8 m/min; the speed of the extension oven is 55.0 m/min; the shrink oven speed was 55.0 m/min.
In example 2, the main control and technical quality indexes of the PVA fiber are as follows:
example 3:
raw materials: plasticizing PVA resin, wherein the polymerization degree is 1750, and the mass ratio of the plasticizer is 42.0%; melting: the temperature feeding area of the twin-screw extruder is 110 ℃; a compression zone of 120 ℃; a melting zone of 130 ℃; a homogenizing and metering area is 135 ℃; and a spinneret assembly 110 ℃.
Spinning: the diameter of the spinneret micropore is 1.0, the length-diameter ratio is 2.5:1, and the drawing ratio of the spinneret is 1.28 times. Circular blowing is carried out at the temperature of 30 ℃ and the wind speed of 1.8 m/min. Multistage drying, hot stretching temperature: a first section of oven 80 ℃; the temperature of the second section of the oven is 100 ℃; the temperature of a third section of the oven is 120 ℃; the fourth section of the oven is at a temperature of 130 ℃; preheating an oven for 180 ℃; an extension oven is 195 ℃; the oven was shrunk 180 ℃. Multistage drying and hot stretching speed: the first section of the oven speed is 6.0 m/min; the second section of the oven speed is 6.2 m/min; the speed of the third section of the oven is 6.4 m/min; the fourth section of the oven speed is 6.6 m/min; the speed of the preheating oven is 6.8 m/min; the extension oven speed is 68.0 m/min; the shrink oven speed was 66.6 m/min.
Example 3 the main control and technical quality indicators of the PVA fibers are as follows:
the invention takes plasticized PVA polymer as raw material, uses desalted water or alcohol compound as plasticizer to greatly reduce the PVA hot-melting temperature, and has the advantages of more environmental protection and cost saving compared with the prior art that the melting temperature is 40-70 ℃ lower when amide compound is used as plasticizer. Utilize the ring blowing mode, the cooling solidification effect is more excellent than the cross-blowing mode among the prior art, and the cooling medium adopt the air can, compare some among the prior art use nitrogen gas, carbon dioxide, oxygen, or its gas mixture form environmental protection and energy saving more. Based on a similar conventional melting waterproof technology, a semi-melting wet process method is adopted, and control parameters among process steps are reasonably set, so that the titer of the PVA fiber is 100-400 dtex.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing polyvinyl alcohol fiber by a semi-melting wet method is characterized by comprising the following steps: the method comprises the following process steps:
s1: blending and plasticizing fiber-forming high polymer PVA resin and an environment-friendly plasticizer according to a certain proportion to obtain plasticized PVA resin;
s2: continuously feeding the plasticized PVA resin to a double-screw extruder through a screw feeder, and completing feeding, compression, melting and homogenizing metering of the plasticized PVA resin through temperature distribution of each area of the double-screw extruder to form molten PVA slurry; filtering the PVA slurry, metering and pressurizing by a metering pump to a spinning assembly, and spinning to obtain nascent fiber;
s3: and finally, preparing the PVA fiber with the titer of 3-600 dtex by the primary fiber through circular air blow molding, multistage drying, hot stretching, oiling and winding.
2. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the parameters of each process in the step S2 are set as follows:
setting the temperature of the double-screw extruder, wherein the feeding area is 105-115 ℃; a compression zone is 115-120 ℃; a melting zone is 125-130 ℃; the homogenization metering area is 130-135 ℃; spinning components are 100-120 ℃;
the diameter of the micropores of the spinning nozzle in the spinning assembly is 0.5-1.25, the length-diameter ratio is 1: 1-3: 1, and the drawing ratio of the spinning nozzle is 0.5-2 times.
3. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the parameters of each process in the step S3 are set as follows:
circularly blowing air at the temperature of 20-40 ℃ and the air speed of 1-3 m/min;
the multistage drying and hot stretching temperature is 50-80 ℃ in a first section of oven; the rear section drying oven is increased according to the temperature gradient of 20-30 ℃; a preheating machine oven is 150-180 ℃; 190-210 ℃ of an stretcher oven; 170-200 ℃ of a shrinker oven;
the multistage drying and hot stretching speed is 0.5-2 times of the first section of oven speed; controlling the passing of tension by the remaining drying ovens, and increasing the speed of the latter section by 0.2-0.5 m/min compared with the speed of the former section; the hot stretching speed is 6-8 times of the speed of the first section of the drying oven; the cooling winding speed is 95-98% of the hot stretching speed;
the surface temperature of the wound fiber after cooling is not higher than 50 ℃.
4. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the polymerization degree of the PVA resin formed by the fiber-forming high polymer in the step S1 is 1700-2600, the alcoholysis degree is 98-99.8 mol%, and the coloration degree is more than or equal to 90%.
5. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the polymerization degree of the plasticized PVA resin in the step S1 is 1700-1800.
6. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the environment-friendly plasticizer is desalted water or alcohol compounds.
7. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: the environment-friendly plasticizer accounts for 30-50% of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
8. The method for preparing polyvinyl alcohol fiber by semi-molten wet process according to claim 7, wherein: the environment-friendly plasticizer accounts for 42.5 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
9. The method for preparing polyvinyl alcohol fiber by semi-molten wet process according to claim 7, wherein: the environment-friendly plasticizer accounts for 43.2 percent of the total amount of reactants participating in the plasticizing reaction in percentage by weight.
10. The method for preparing polyvinyl alcohol fiber by semi-molten wet method according to claim 1, wherein: and finally preparing the PVA fiber with the titer of 100-400 dtex in the S3.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB895390A (en) * | 1958-08-19 | 1962-05-02 | Kurashiki Rayon Kk | A method of manufacturing synthetic filaments of polyvinyl alcohol of high quality |
| CN102605446A (en) * | 2012-03-22 | 2012-07-25 | 上海罗洋新材料科技有限公司 | Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre |
| CN102776598A (en) * | 2012-03-22 | 2012-11-14 | 上海罗洋新材料科技有限公司 | Preparation method of melt spun high-strength high-modulus polyvinyl alcohol fibers |
| CN102776597A (en) * | 2012-03-22 | 2012-11-14 | 上海罗洋新材料科技有限公司 | High-strength and high-modulus polyvinyl alcohol fiber and melt spinning method of high-strength and high-modulus polyvinyl alcohol fiber |
| CN107287675A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of vinal and preparation method thereof |
-
2021
- 2021-05-13 CN CN202110523616.7A patent/CN113062004A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB895390A (en) * | 1958-08-19 | 1962-05-02 | Kurashiki Rayon Kk | A method of manufacturing synthetic filaments of polyvinyl alcohol of high quality |
| CN102605446A (en) * | 2012-03-22 | 2012-07-25 | 上海罗洋新材料科技有限公司 | Annular blowing cooling solidification process method for preparing polyvinyl alcohol fibre |
| CN102776598A (en) * | 2012-03-22 | 2012-11-14 | 上海罗洋新材料科技有限公司 | Preparation method of melt spun high-strength high-modulus polyvinyl alcohol fibers |
| CN102776597A (en) * | 2012-03-22 | 2012-11-14 | 上海罗洋新材料科技有限公司 | High-strength and high-modulus polyvinyl alcohol fiber and melt spinning method of high-strength and high-modulus polyvinyl alcohol fiber |
| CN107287675A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of vinal and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 姜猛进 等: "《高强高模聚乙烯醇纤维》", 30 June 2017, 国防工业出版社 * |
| 毛应鹏: "聚乙烯醇的熔融纺丝", 《合成纤维》 * |
| 王洪学等: "二元复配增塑剂对热塑性聚乙烯醇性能的影响", 《合成树脂及塑料》 * |
| 钱知勉: "《塑料性能应用手册》", 31 March 1987, 上海科学技术文献出版社 * |
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