CN110306335A - Moisture-absorption polyacrylonitrile fiber - Google Patents
Moisture-absorption polyacrylonitrile fiber Download PDFInfo
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- CN110306335A CN110306335A CN201910386841.3A CN201910386841A CN110306335A CN 110306335 A CN110306335 A CN 110306335A CN 201910386841 A CN201910386841 A CN 201910386841A CN 110306335 A CN110306335 A CN 110306335A
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Abstract
The present invention provides moisture-absorption polyacrylonitrile fiber, belong to chemical fiber field, moisture-absorption polyacrylonitrile fiber is obtained by following steps: mixed liquor of the polyacrylonitrile fibre containing NaOH solution, basic amine group acid solution is hydrolyzed, it is 6-7 that pH is neutralized to after cooling, add cross-linking agent solution crosslinking, cleaning, regain >=3.64% of polyacrylonitrile fibre obtained, higher than the 375.26% of non-hydrophilic modifying acrylic fiber.Preparation method of the present invention enables to the carboxyl in basic amino acid being capable of and Al common with acrylic fibers in subsequent cross-linking process3+It is connected in, retain basic amino acid backbone amino and pendant basic group, improve the water solubility and electropositive of acrylic fibers, assign the certain bacteriostatic activity of acrylic fibers and persistently, color, form and the mechanical performance of poly- propionitrile fiber can be preferably kept, polyacrylonitrile fibre obtained is with the permanent antibiotic property of duration, the moisture-absorption polyacrylonitrile fiber of preferable form and mechanical performance.
Description
Technical field
The invention belongs to chemical fiber fields, and in particular to moisture-absorption polyacrylonitrile fiber.
Background technique
Polyacrylonitrile fibre (abbreviation trade name nitrile opinion) is a kind of important chemical fibre kind and textile raw material, it is after washing
By the third-largest synthetic fibers kind in China after, nylon, has the characteristics that excellent warmth retention property, dyeability and imitative hair, have
The title of artificial wool is widely used in the fields of taking such as knitted underwear, woollen blanket, artificial furs.But with people's living standard
Continuous improvement and clothing design it is increasingly developed, warming has no longer been the unitary request of clothes, and people are to its comfort level, function
Property and security requirement are higher and higher.The gender gap comfortable and easy to wear of different fibrous material clothes is related with the moisture pick-up properties of fiber,
Moisture pick-up properties can be indicated with official regain.The official regain of natural fiber is about 8~15%, and polyacrylonitrile fibre is only
2%, serious defect is shown in the performance relevant to human body skin-friendly such as hygroscopicity, penetrability, makes its manufactured clothing
Dress has feeling of oppression and heat, sweat to be not easy to be absorbed and distribute, and static behaviour is strong, generally requires additional functionality processing or spin after reducing to be blended
Ratio not only increases processing cost, but also the durability for the treatment of effect is lower, thus greatly reduces the clothes of polyacrylonitrile fibre
It is more limited in certain field applications for thering is antistatic property to require with performance.Influencing the hygroscopic principal element of fiber usually has parent
The polyacrylonitrile fibres such as water base group's effect, crystallization situation, impurity, specific surface area are gathered by the height that Raolical polymerizable is formed
The characteristics of object, all kinds of polyacrylonitrile molecule structures, is all made of acrylonitrile and other vinyl monomer random copolymerizations, linear big
Molecular backbone is mainly joined end to end by acrylonitrile unit.It is mutually exclusive between adjacent cyano on same macromolecular chain, it is adjacent
Cyano and a hydrogen atom form hydrogen bond and attract each other between macromolecular chain.The interaction of this repulsion and gravitation makes macromolecular master
Chain is distorted, and forms random coil shape three-dimensional conformation in space.
For textile fabric, hydrophily refers to the ability that fiber absorbs moisture and conveys moisture to adjacent fibre, presses
Hygroscopicity fibre and moisture-absorbing fibre can be subdivided into according to mechanism.People have conducted extensive research to improve polypropylene nitrile fiber at present
Hydrophilicity, so that it is had the hot wet migration of natural fiber.Such as the invention of 103233291 B of Authorization Notice No. CN is special
Benefit discloses a kind of preparation method of moisture-absorption polyacrylonitrile fiber, comprises the steps of that the fiber (1), which is made, uses alkalinous metal
Acrylonitrile copolymer is hydrolyzed in saline solution；(2) solvent precipitation is used, adjusts pH value after filtering；(3) spin solvent is used
Obtained hydrolysate polyacrylonitrile is deployed into hydrolyzed polyacrylonitrile stoste；(4) by the hydrolyzed polyacrylonitrile stoste temperature adjustment, with
The polyacrylonitrile matrix routinely produced is sufficiently mixed uniformly, and moisture absorption polyacrylonitrile matrix is prepared；(5) by stoste in polypropylene
Solidification forming is squeezed out on nitrile wet spinning production line, preliminary draft, washing, hydrophilicity-imparting treatment, hot gas spring, densification-crosslinking, is determined
Type oils and moisture-absorption polyacrylonitrile fiber is made after baking process.A kind of system of moisture-absorption polyacrylonitrile fiber provided by above-mentioned
Preparation Method not only has good moisture pick-up properties, but also uniformity is good, and durability is good, is not limited by fibre number, length,
High production efficiency.The patent of invention of 103205823 B of Authorization Notice No. CN discloses a kind of preparation of hydrophilic polyacrylonitrile fiber
Method, it is characterised in that comprise the steps of be made the fiber (1) with alkalinous metal saline solution to acrylonitrile copolymer into
Row hydrolysis process；(2) acid for adjusting pH value is added to 4~7 in the hydrolyzate solvent precipitation that will be obtained after filtering；(3) molten with spinning
Obtained hydrolysate polyacrylonitrile is deployed into hydrolyzed polyacrylonitrile stoste by agent；(4) by the hydrolyzed polyacrylonitrile stoste temperature adjustment,
It is sufficiently mixed with the polyacrylonitrile matrix that routinely produces with certain mass ratio uniform, hydrophilic polyacrylonitrile stoste is prepared；(5)
By stoste through squeezing out solidification forming, preliminary draft, washing, hot gas spring, densification-friendship on polyacrylonitrile wet spinning production line
Join, be formed, oiling and hydrophilic polyacrylonitrile fiber is made after baking process.A kind of preparation side of above-mentioned hydrophilic polyacrylonitrile fiber
Method not only has good moisture pick-up properties, but also uniformity is good, and durability is good, is not limited by fibre number, length, produces
It is high-efficient.
Summary of the invention
The purpose of the present invention is to provide a kind of carboxyl enabled in basic amino acid in subsequent cross-linking process energy
It is enough with acrylic fibers jointly and Al3+Be connected in, retain basic amino acid backbone amino and pendant basic group, improve acrylic fibers water solubility and
Electropositive assigns the certain bacteriostatic activity of acrylic fibers and persistently, can preferably keep color, form and the mechanicalness of poly- propionitrile fiber
The preparation method of the moisture-absorption polyacrylonitrile fiber of energy.
The technical solution that the present invention is taken to achieve the above object are as follows:
The preparation method of moisture-absorption polyacrylonitrile fiber, including polyacrylonitrile fibre is used and contains NaOH solution, basic amine group
The mixed liquor of acid solution hydrolyzes, and it is 6-7 that pH is neutralized to after cooling, adds cross-linking agent solution crosslinking, cleaning.
The present invention carries out hydrophilic modifying to acrylic fibers using alkali-organic solvent method, easy to operate, to equipment without particular/special requirement,
Reaction condition is mild；A large amount of OH- can be contained in solution, necleophilic reaction occurs in the positively charged carbon atom of easy attack.Solution
In hydroxide ion attack-CN, and form covalent bond with carbon atom, it is former that negative electrical charge has been transferred to the high nitrogen of cloud density
On son, the intermediate with electronegativity is generated, which has very strong nucleophilie nucleus ability, can continue to occur with adjacent cyano
Nucleophilic addition generates six-membered cyclic structure, ultimately generates the hexatomic ring of a series of covalent bond, the condition existing for water
Under, intermediate, hexatomic ring can be in conjunction with water, and tautomerism occurs, hydrophilic radical-CONH2, then amide group is in aqueous slkali
The middle attack continued by hydroxide ion, hydrolysis generates hydrophilic radical-COOH and-COONa, and releases ammonia；Subsequent crosslinking
Carboxyl after reaction on different molecular chain is crosslinked by cross-linking agent together, forms mesh space structure, and this structure enhances
The water conservation of acrylic fibers, moisture pick-up properties are saved in not easy to lose in fiber, and hydrolyzed polyacrylonitrile after so that moisture is entered fiber surface
Strength it is preferable, will not influence the use during textile process.Basic amino acid used in hydrolytic process includes arginine, relies
Propylhomoserin, histidine, the hydroxyl radical negative ion that the hydrolysis of one side basic amino acid generates are more than the amino acid of hydrogen cation, Neng Gouti
OH in high solution-And OH in NaOH-Gain effect is played, the fracture of three keys in-CN is collectively promoted, improves containing for hydrophilic radical
Amount, and then increase the hydrophilicity of acrylic fibers；Carboxyl in another aspect basic amino acid can be in subsequent cross-linking process
Acrylic fibers are common and Al3+Be connected in, to retain basic amino acid backbone amino and pendant basic group, improve acrylic fibers water solubility and
Electropositive assigns acrylic fibers certain bacteriostatic activity, and basic amino acid backbone amino can steadily exist with pendant basic group
In poly- propionitrile fibre structure, lasting antibacterial efficacy is able to maintain in aqueous solution, this external enwergy preferably keeps poly- third
The form and mechanical performance of nitrile fiber, meet further research and development.
Preferably, the concentration of NaOH solution is 3.8-5.6%, the concentration of basic amine group acid solution is 0.5-1.6%.
Preferably, NaOH solution and the volume ratio of basic amine group acid solution are 100:3-10.
Preferably, the bath raio of hydrolysis is 1:20-28, and hydrolysis temperature is 70-95 DEG C, hydrolysis time 8-14min.
Preferably, ethyl alcohol and mannitol are added in hydrolytic process.The addition of ethyl alcohol and mannitol can not only be with further
The hydrolysis for promoting cyano in acrylic fibers molecule, makes more cyan-hydrolysis carboxyls, improves the regain of acrylic fibers；And it can promote
The hexatomic ring intermediate that hydrolytic process re-generates further generates amide group, reduces by six in hydrolysate-hydrolyzed polyacrylonitrile
The presence of member ring intermediate, to maintain the color of acrylic fiber, while the ammonia that can be released in water resistance sealing solution preocess
It reacts with unhydrolysed cyano and generates amidino groups, further maintain the whiteness of fiber.
Preferably, cross-linking agent solution is formalin and/or aluminum hydroxide solution and/or liquor alumini chloridi.
Preferably, cross-linking agent solution is the AlCl that concentration is 0.05-0.07g/L3·6H2O solution, crosslinking temperature 90-
100 DEG C, time 20-50min.
It is another object of the present invention to provide a kind of regain >=3.64%, the antibiotic property for having duration permanent,
The moisture-absorption polyacrylonitrile fiber of preferable form and mechanical performance.
The technical solution that the present invention is taken to achieve the above object are as follows:
Moisture-absorption polyacrylonitrile fiber is made by the preparation method of above-mentioned moisture-absorption polyacrylonitrile fiber.
Preferably, regain >=3.64% of polyacrylonitrile fibre.Higher than the 375.26% of non-hydrophilic modifying acrylic fiber.
Preferably, polyacrylonitrile fibre is fibre bundle, fiber cloth, fiber filament, fibrofelt or fabric.
Compared with prior art, the invention has the benefit that
The preparation method of moisture-absorption polyacrylonitrile fiber of the present invention can weaken active force between cellulosic molecule, reduce cellulose point
The bond energy of son, is easier to it with hydrogen ion ining conjunction with, thus the finally raising mechanical property of moisture-absorption polyacrylonitrile fiber and soft
It is soft；The preparation method of moisture-absorption polyacrylonitrile fiber of the present invention is enhanced between antibacterial agent and the cellulosic molecule of base fabric by chemical bond
Being firmly combined property, antibacterial agent is fixed on during subsequent curing process and is formed by film, antibacterial agent will not be easily
It is fallen off by external force, improves the antibacterial stability and persistence of moisture-absorption polyacrylonitrile fiber；Moisture absorption polypropylene of the present invention
The preparation method of nitrile fiber can promote TiO2Crystallinity, increase its crystallite dimension, increase specific surface area, inhibit TiO2
The conversion of crystal form, so that TiO2Form it is more stable, and then improve the duration of action of the nano self-cleaning agent；System of the present invention
Preparation Method obtain moisture-absorption polyacrylonitrile fiber not only have preferable mechanical property, flexibility, gas permeability, antibacterial stability and
Persistence, automatically cleaning stability and persistence.
Present invention employs above-mentioned technical proposals to provide moisture-absorption polyacrylonitrile fiber, compensates for the deficiencies in the prior art, if
Meter is rationally, easy to operate.
Specific embodiment
Hydrophilic modifying is carried out to acrylic fibers using alkali-organic solvent method, it is easy to operate, to equipment without particular/special requirement, react item
Part is mild；A large amount of OH- can be contained in solution, necleophilic reaction occurs in the positively charged carbon atom of easy attack.Hydrogen in solution
Oxygen radical ion attack-CN, and covalent bond is formed with carbon atom, negative electrical charge has been transferred on the high nitrogen-atoms of cloud density,
The intermediate with electronegativity is generated, which has very strong nucleophilie nucleus ability, can continue that nucleophilic occurs with adjacent cyano
Addition reaction generates six-membered cyclic structure, ultimately generates the hexatomic ring of a series of covalent bond, under the conditions of existing for the water, in
Mesosome, hexatomic ring can be in conjunction with water, and tautomerism occurs, hydrophilic radical-CONH2, then amide group is relayed in aqueous slkali
The continuous attack by hydroxide ion, hydrolysis generates hydrophilic radical-COOH and-COONa, and releases ammonia；Subsequent cross-linking reaction
The carboxyl on different molecular chain is crosslinked by cross-linking agent together later, forms mesh space structure, and this structure enhances acrylic fibers
Water conservation, moisture pick-up properties, be saved in not easy to lose in fiber after so that moisture is entered fiber surface, and hydrolyzed polyacrylonitrile is strong
Power is preferable, will not influence the use during textile process.
The present inventor conducts in-depth research the hydrolysis process of polyacrylonitrile fibre, by control alkaline concentration,
Water-bath ratio, hydrolysis temperature and time, crosslinking agent solubility and crosslinking temperature, crosslinking time obtain regain >=3.64%, have and hold
The permanent antibiotic property of continuous property, the moisture-absorption polyacrylonitrile fiber of preferable form and mechanical performance.
The preparation method of moisture-absorption polyacrylonitrile fiber of the invention, including,
Step 1: polyacrylonitrile fibre is placed in reactor, by bath raio be 1:20-28 be added containing concentration be 3.8-
The mixed liquor of 5.6% NaOH solution, the basic amine group acid solution that concentration is 0.5-1.6%, wherein NaOH solution and alkaline ammonia
The volume ratio of base acid solution is 100:3-10, hydrolyzes 8-14min at being 70-95 DEG C in temperature；
Step 2: it is 6-7 by pH is neutralized to after hydrolysis cooling, adds cross-linking agent solution crosslinking, finally cleaned with clear water,
Gained moisture-absorption polyacrylonitrile fiber is dried at 100-110 DEG C.
Basic amino acid used in hydrolytic process includes arginine, lysine, histidine, the hydrolysis of one side basic amino acid
The hydroxyl radical negative ion of generation is more than the amino acid of hydrogen cation, can be improved OH in solution-And OH in NaOH-Gain is played to make
With collectively promoting the fracture of three keys in-CN, improve the content of hydrophilic radical, and then increase the hydrophilicity of acrylic fibers；Another party
Carboxyl in the basic amino acid of face being capable of and Al common with acrylic fibers in subsequent cross-linking process3+It is connected in, to retain basic amine group
Sour backbone amino and pendant basic group improve the water solubility and electropositive of acrylic fibers, assign acrylic fibers certain bacteriostatic activity, and alkali
Acidic amino acid backbone amino and pendant basic group can steadily be present in poly- propionitrile fibre structure, even if in aqueous solution
It is able to maintain lasting antibacterial efficacy, this external enwergy preferably keeps the form and mechanical performance of poly- propionitrile fiber, meets further
Research and development.
In order to improve the regain of polyacrylonitrile fibre and maintain the whiteness of acrylic fiber, moisture absorption polyacrylonitrile of the invention
Ethyl alcohol and mannitol are added in hydrolytic process in the preparation method of fiber.The addition of ethyl alcohol and mannitol can not only follow up one
Step promotes the hydrolysis of cyano in acrylic fibers molecule, makes more cyan-hydrolysis carboxyls, improves the regain of acrylic fibers；And it can promote
The hexatomic ring intermediate that water inlet solution preocess re-generates further generates amide group, reduces in hydrolysate-hydrolyzed polyacrylonitrile
The presence of hexatomic ring intermediate, to maintain the color of acrylic fiber, while the ammonia that can be released in water resistance sealing solution preocess
Gas and unhydrolysed cyano react and generate amidino groups, further maintain the whiteness of fiber.Preferably, ethyl alcohol and mannitol
Additional amount is respectively 4-7 times and 0.04-0.15 times of polyacrylonitrile fibre weight.The addition of ethyl alcohol and mannitol within the scope of this
Amount can improve the regain of polyacrylonitrile fibre to the maximum extent and maintain the whiteness of acrylic fiber.
Polyacrylonitrile fibre hydrolysis after neutralizing, carries out crosslinking Treatment to it, to improve the moisture pick-up properties of fabric.This hair
The cross-linking agent solution used in the preparation method of bright moisture-absorption polyacrylonitrile fiber is formalin and/or aluminum hydroxide solution
And/or liquor alumini chloridi.Preferably, cross-linking agent solution is the AlCl that concentration is 0.05-0.07g/L3·6H2O solution, crosslinking temperature
Degree is 90-100 DEG C, time 20-50min.Aluminium chloride is soluble in, is soluble in the organic solvents such as ethyl alcohol, aluminium chloride non-toxic and safe
Coefficient is high.Wherein, the solid-liquid ratio of polyacrylonitrile fibre and cross-linking agent solution is 1:0.3-0.4 (g/mL).
Moisture-absorption polyacrylonitrile fiber of the invention is made by the preparation method of above-mentioned moisture-absorption polyacrylonitrile fiber.
Regain >=3.64% of polyacrylonitrile fibre of the invention.Higher than non-hydrophilic modifying acrylic fiber
375.26%.
Polyacrylonitrile fibre of the invention is fibre bundle, fiber cloth, fiber filament, fibrofelt or fabric.
In the following, being described further in conjunction with specific embodiments to embodiment of the present invention.
Embodiment 1:
The preparation method of moisture-absorption polyacrylonitrile fiber, including,
Step 1: polyacrylonitrile fibre beam being placed in reactor, be that 1:20 is added by bath raio containing concentration is 3.8%
NaOH solution, concentration be 0.5% arginine solution mixed liquor, add 4 times of polyacrylonitrile fibre Shu Chongliang ethyl alcohol and
The mannitol that 0.04 times of polyacrylonitrile fibre Shu Chongliang, wherein the volume ratio of NaOH solution and arginine solution is 100:3, in temperature
Degree is to hydrolyze 8min at 70 DEG C；
Step 2: will hydrolysis it is cooling after to be neutralized to pH be 6, then be 1:0.3 (g/mL) addition concentration by solid-liquid ratio be 0.05g/
The AlCl of L3·6H2O solution is crosslinked 20min under the conditions of at a temperature of 90 °C, is finally cleaned with clear water, by gained moisture absorption poly- third
Alkene nitrile fibre bundle is in 100 DEG C of drying to get moisture-absorption polyacrylonitrile fiber beam.
Embodiment 2:
The preparation method of moisture-absorption polyacrylonitrile fiber, including,
Step 1: polyacrylonitrile fibre silk being placed in reactor, be that 1:26 is added by bath raio containing concentration is 5.0%
NaOH solution, concentration be 1.2% lysine solution mixed liquor, add 5 times of polyacrylonitrile fibre silk weight ethyl alcohol and
The mannitol of 0.1 times of polyacrylonitrile fibre silk weight, wherein NaOH solution and the volume ratio of lysine solution are 100:6, in temperature
Degree is to hydrolyze 10min at 85 DEG C；
Step 2: will hydrolysis it is cooling after to be neutralized to pH be 6.5, then by solid-liquid ratio be that 1:0.35 (g/mL) addition concentration is
The AlCl of 0.06g/L3·6H2O solution is crosslinked 35min under conditions of temperature is 95 DEG C, is finally cleaned with clear water, gained is inhaled
Wet polyacrylonitrile fibre silk is in 105 DEG C of drying to get moisture-absorption polyacrylonitrile fiber silk.
Embodiment 3:
The preparation method of moisture-absorption polyacrylonitrile fiber, including,
Step 1: polyacrylonitrile fibre being arranged in reactor, be that 1:28 is added by bath raio containing concentration is 5.6%
NaOH solution, concentration be 1.6% histidine solution mixed liquor, add 7 times of polyacrylonitrile fibre cloth weight ethyl alcohol and
The mannitol of 0.15 times of polyacrylonitrile fibre cloth weight, wherein NaOH solution and the volume ratio of histidine solution are 100:10,
Temperature is to hydrolyze 14min at 95 DEG C；
Step 2: will hydrolysis it is cooling after to be neutralized to pH be 7, then be 1:0.4 (g/mL) addition concentration by solid-liquid ratio be 0.07g/
The AlCl of L3·6H2O solution is crosslinked 50min under conditions of temperature is 100 DEG C, is finally cleaned with clear water, gained moisture absorption is gathered
Dralon cloth is in 110 DEG C of drying to get moisture-absorption polyacrylonitrile fiber cloth.
Embodiment 4:
In order to further increase the mechanical property and anti-microbial property of moisture-absorption polyacrylonitrile fiber, the technical side advanced optimized
Case are as follows:
The preparation method of moisture-absorption polyacrylonitrile fiber, including,
Step 1: polyacrylonitrile fibre silk being placed in reactor, be that 1:26 is added by bath raio containing concentration is 5.0%
NaOH solution, concentration be 1.2% lysine solution mixed liquor, add 5 times of polyacrylonitrile fibre silk weight ethyl alcohol and
The mannitol of 0.1 times of polyacrylonitrile fibre silk weight, wherein NaOH solution and the volume ratio of lysine solution are 100:6, in temperature
Degree is to hydrolyze 10min at 85 DEG C；
Step 2: will hydrolysis it is cooling after to be neutralized to pH be 6.5, then by solid-liquid ratio be that 1:0.35 (g/mL) addition concentration is
The AlCl of 0.06g/L3·6H2O solution is crosslinked 35min under conditions of temperature is 95 DEG C, is finally cleaned with clear water, gained is inhaled
Wet polyacrylonitrile fibre silk is dried at 105 DEG C, and then the gamma-ray irradiation under conditions of power of irradiation bomb is 8.0kGy/h, inhales
Receiving dosage is 50-80kGy to get moisture-absorption polyacrylonitrile fiber silk.Gamma-rays is that a kind of wavelength is most short, the highest electromagnetism of energy
Wave, one of high energy particle can just make irradiated material generate many excitation molecule or ion, and in radiative process
There are many active particle type of middle generation, therefore, some heat chemistrys and the unapproachable chemical reaction of photochemistry, using gamma-rays
Processing may be implemented.The preparation method is subsequent to take gamma-ray irradiation, can induce and be formed certainly on polyacrylonitrile fibre molecule
By base, it can further promote further perfect, the raising cross-linked three D reticular point of cross-linking reaction on polyacrylonitrile fibre molecule
The stability of minor structure, and mainly based on intermolecular crosslinking, radiation-induced cross-linking products occur mainly in amorphous area, and
Influence to crystal region is little, to further enhance the water conservation of acrylic fibers, moisture pick-up properties and anti-microbial property, and can enhance water
Solve the mechanical property of polyacrylonitrile；Irradiation can't destroy the crystalline structure of PAN simultaneously, improve fiber core-skin uniformity and
Mechanical property.
Comparative example 1:
The difference of this comparative example and the technical solution of embodiment 2 is: only containing in this comparative example hydrolysis mixed liquor
NaOH solution.
Comparative example 2:
The difference of this comparative example and the technical solution of embodiment 2 is: the hydrolysis of this comparative example is depended on containing only in mixed liquor
Propylhomoserin solution.
Comparative example 3:
The difference of this comparative example and the technical solution of embodiment 3 is: ethyl alcohol is only added with mixed liquor in the hydrolysis of this comparative example.
Comparative example 4:
The difference of this comparative example and the technical solution of embodiment 3 is: sweet dew is only added with mixed liquor in the hydrolysis of this comparative example
Alcohol.
Comparative example 5:
The difference of this comparative example and the technical solution of embodiment 3 is: only containing in this comparative example hydrolysis mixed liquor
Ethyl alcohol is only added with mixed liquor in NaOH solution, hydrolysis.
Test example 1:
The performance test of moisture-absorption polyacrylonitrile fiber
1. regain: it is measured by GB/T 6503-2017 method:
Moisture-absorption polyacrylonitrile fiber is put into climatic chamber, under standard atmospheric conditions (20 DEG C of temperature, humidity 65%)
Balance 24 hours or more, claims its weight in wet base, calculates the regain of moisture-absorption polyacrylonitrile fiber, calculation method:
W (%)=(M1–M2)/M1× 100%；
In formula: W indicates regain, M1Indicate quality before absorbing water, M2Indicate quality after absorbing water.The results are shown in Table 1.
2. mechanical property: it is measured by GB/T 14344-2008 method:
Test apparatus: YG061F type electronics single yarn tester；
Experimental condition: clamping length 500mm, tensile speed are used relative to the sample 100% constant drawing extended as former state
Stretch speed.Pre-tension is 10cN, and temperature is 20 DEG C, relative humidity 65%, is averaged after test 30 times；
Characteristic index: ultimate strength, breaking strength, elongation at break.The results are shown in Table 1.
The performance test results of 1 moisture-absorption polyacrylonitrile fiber of table
| Project | Regain (%) | Ultimate strength (cN) | Breaking strength (cNtex-1) | Elongation at break (%) | Color |
| Embodiment 2 | 3.72 | 327 | 17.9 | 4.5 | White |
| Embodiment 4 | 3.87 | 346 | 19.2 | 4.8 | White |
| Comparative example 1 | 3.54 | 287 | 12.4 | 5.8 | White |
| Comparative example 2 | 1.72 | 271 | 13.0 | 6.0 | White |
| Comparative example 3 | 3.34 | 199 | 11.0 | 6.7 | It is yellowish |
| Comparative example 4 | 2.89 | 210 | 10.8 | 6.7 | It is yellowish |
| Comparative example 5 | 1.63 | 193 | 10.3 | 6.9 | It is yellowish |
| Former polyacrylonitrile fibre | 0.97 | 330 | 18.6 | 4.6 | White |
As shown in Table 1, the regain of moisture-absorption polyacrylonitrile fiber made from the embodiment of the present invention 2 and mechanical property are much good
In comparative example 1, comparative example 2 and comparative example 5, this illustrates that the presence of hydrolytic process neutral and alkali amino acid can increase the hydrophilic of acrylic fibers
Performance preferably keeps the form and mechanical performance of poly- propionitrile fiber；Moisture-absorption polyacrylonitrile fiber made from the embodiment of the present invention 2
Regain and mechanical property and color can be far better than comparative example 3, comparative example 4 and comparative example 5, this illustrates ethyl alcohol in hydrolytic process
Addition with mannitol can not only improve the regain of acrylic fibers, and be able to maintain that the color of acrylic fiber；The present invention is implemented
The regain and mechanical property of moisture-absorption polyacrylonitrile fiber made from example 4 are better than embodiment 2, this shows subsequent to take gamma-ray irradiation
Water conservation, the moisture pick-up properties of acrylic fibers can be further enhanced, and the mechanical property of hydrolyzed polyacrylonitrile can be enhanced.
3. antibiotic property and washing fastness: according to succusion (GB/T20944.3-2008 " evaluation of antibacterial textile performance "
Third portion) it is measured, the objective microbe of test includes Escherichia coli, staphylococcus aureus, Candida albicans and black
Aspergillus.Anti-microbial property test selects former polyacrylonitrile fibre as control fabric.Antibiotic rate is calculated according to the following formula:
R=(B-A)/B × 100%；
Wherein, R is the antibiotic rate of moisture-absorption polyacrylonitrile fiber；B is the clump count on former poly- propionitrile fibre solid culture medium；
A is the clump count on moisture-absorption polyacrylonitrile fiber solid medium.Mould proof rank is judged by following standard: 0 grade-
Aspergillus niger is not grown on solid medium；The growth area of aspergillus niger is less than 10% on 1 grade-solid medium；The training of 2 grades-solid
The growth area for supporting ?aspergillus on base is greater than 10%.
Washing fastness is measured according to GB/T8629-2001 " one textile testing of textile with home washings and drying program "
Energy.Sequentially added first into washing machine fiber to be measured (0.2kg, 40cm × 40cm), WOB standard detergent (AATCC1993,
2g/L) (50 DEG C, hardness is 20mg/kg CaCO with enough water3).Then start washing machine, dry 6min after washing 15min.
After washing 30 times and 50 times as procedure described above, fabric sample is placed in 60 DEG C of drying box and is sufficiently dried.Finally,
According to the succusion (GB/T20944.3-2008 " evaluation of antibacterial textile performance " third portion) of antibacterial fabric performance test,
Anti-microbial property test is carried out to washing 30 times and 50 times fabric samples.
On former polyacrylonitrile fibre solid medium and comparative example 1, the clump count of comparative example 5 are quite a lot of, with blank indifference
Different, embodiment 2, embodiment 4 and comparative example 2, comparative example 3, comparative example 4 obtain moisture-absorption polyacrylonitrile fiber and resist to Escherichia coli
Bacterium rate respectively reaches 95.01%, 98.43% and 94.23%, 94.09%, 94.16%；To the antibiotic rate of staphylococcus aureus
Respectively reach 96.42%, 99.11% and 95.87%, 96.07%, 95.67%；The antibiotic rate of Candida albicans is respectively reached
95.57%, 99.24% and 95.19%, 94.87%, 94.88%.In addition, embodiment 2, embodiment 4 and comparative example 2, comparative example
3, on 4 moisture-absorption polyacrylonitrile fiber solid medium of comparative example the growth Line Integral of aspergillus niger be not 0%, 0% and 1.3%,
0.8%, 0.7%, embodiment 2, embodiment 4 and comparative example 2, comparative example 3, the mould proof grade of 4 moisture-absorption polyacrylonitrile fiber of comparative example
0 grade, 0 grade and 1 grade, 1 grade, 1 grade are not respectively reached.As washing times increase to 30 times and 50 times, embodiment 2 and comparison from 0
Example 2, comparative example 3, the Escherichia coli of 4 moisture-absorption polyacrylonitrile fiber of comparative example, staphylococcus aureus and Candida albicans survival
Quantity, which has, to be increased, but Aspergillus Niger Growth area is constant, to the antibiotic rates of Escherichia coli respectively from 95.01% and 94.23%,
94.09%, 94.16% it is reduced to 94.27%, 94.06%, 93.26%, 93.56%；To the antibiotic rate of staphylococcus aureus
It is reduced to 94.67%, 94.24%, 94.56%, 93.79% from 96.42%, 95.87%, 96.07%, 95.67%, to white
The antibiotic rate of candida albicans is reduced to 94.26% from 95.57%, 95.19%, 94.87%, 94.88%, 93.55%, 93.32%,
93.28%；The mould proof rank of fabric is not caused to reduce；The Escherichia coli of 4 moisture-absorption polyacrylonitrile fiber of embodiment, golden yellow grape
Coccus and Candida albicans amount of survival do not increase, and Aspergillus Niger Growth area is constant, are still 0%, to the mould proof rank of fabric
It does not cause to reduce, is still 1 grade.The above result shows that former polyacrylonitrile fibre itself does not have an anti-microbial property, comparative example 1 and right
The moisture-absorption polyacrylonitrile fiber that ratio 5 obtains also does not have an anti-microbial property, and the moisture-absorption polyacrylonitrile fiber that embodiment 4 obtains
Antibacterial effect and wash resistant effect are better than embodiment 2 and comparative example 2, comparative example 3, comparative example 4, this shows in hydrolytic process
The presence of basic amine group acid solution can assign acrylic fibers certain bacteriostatic activity, and basic amino acid backbone amino and pendant basic
Group can steadily be present in poly- propionitrile fibre structure, and lasting antibacterial efficacy is able to maintain in aqueous solution；Then
It is continuous to take gamma-ray irradiation, the anti-microbial property of acrylic fibers can be further enhanced.
The prior art of routine techniques dawn known to those skilled in the art in above-described embodiment, therefore herein no longer in detail
It repeats.
The above embodiments are only used to illustrate the present invention, and not limitation of the present invention, the ordinary skill people of this field
Member can also make a variety of changes and modification without departing from the spirit and scope of the present invention.Therefore, all equivalent
Technical solution also belong to scope of the invention, scope of patent protection of the invention should be defined by the claims.
Claims (10)
1. the preparation method of moisture-absorption polyacrylonitrile fiber, it is characterised in that: including by polyacrylonitrile fibre use containing NaOH solution,
The mixed liquor of basic amine group acid solution hydrolyzes, and it is 6-7 that pH is neutralized to after cooling, adds cross-linking agent solution crosslinking, cleaning.
2. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1, it is characterised in that: the NaOH solution
Concentration be 3.8-5.6%, the concentration of basic amine group acid solution is 0.5-1.6%.
3. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1 or 2, it is characterised in that: the NaOH
The volume ratio of solution and basic amine group acid solution is 100:3-10.
4. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1, it is characterised in that: the bath of the hydrolysis
Than for 1:20-28, hydrolysis temperature is 70-95 DEG C, hydrolysis time 8-14min.
5. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1 or 2, it is characterised in that: the hydrolysis
Ethyl alcohol and mannitol are added in the process.
6. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1, it is characterised in that: the crosslinking agent is molten
Liquid is formalin and/or aluminum hydroxide solution and/or liquor alumini chloridi.
7. the preparation method of moisture-absorption polyacrylonitrile fiber according to claim 1 or 6, it is characterised in that: the crosslinking
Agent solution is the AlCl that concentration is 0.05-0.07g/L3·6H2O solution, crosslinking temperature are 90-100 DEG C, time 20-50min.
8. moisture-absorption polyacrylonitrile fiber, it is characterised in that: by the described in any item moisture-absorption polyacrylonitrile fibers of claim 1-7
Preparation method is made.
9. moisture-absorption polyacrylonitrile fiber according to claim 8, it is characterised in that: the regain of the polyacrylonitrile fibre
>=3.64%.
10. moisture-absorption polyacrylonitrile fiber according to claim 8 or claim 9, which is characterized in that the polyacrylonitrile fibre is fibre
Tie up beam, fiber cloth, fiber filament, fibrofelt or fabric.
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