CN105155015A - Antistatic acrylic fiber and preparation method thereof - Google Patents
Antistatic acrylic fiber and preparation method thereof Download PDFInfo
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- CN105155015A CN105155015A CN201510452183.5A CN201510452183A CN105155015A CN 105155015 A CN105155015 A CN 105155015A CN 201510452183 A CN201510452183 A CN 201510452183A CN 105155015 A CN105155015 A CN 105155015A
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Abstract
The invention relates to an antistatic acrylic fiber and a preparation method thereof. The preparation method comprises the following steps: drying and screening polyacrylonitrile (PAN) so as to obtain treated PAN; mixing the treated PAN, graphene oxide (GO) and a solvent so as to obtain a spinning solution; and subjecting the spinning solution to vacuum pumping filtration and deaeration, wet spinning, shaping and drying so as to obtain the antistatic acrylic fiber. The acrylic fiber prepared by using the method has excellent mechanical properties, improved mechanical properties and good antistatic performance and can be applied to antistatic fabrics.
Description
Technical field
The invention belongs to antistatic fibre and preparation field thereof, particularly a kind of antistatic acrylic fiber fiber and preparation method thereof.
Background technology
Textiles easily produces electrostatic because rubbing and responding in production and processing with in using.The charge buildup phenomenon of the general lower synthetic fiber goods of regain is more remarkable.In production, the electrification phenomenon of textile material often can cause Filament-wound Machine or blocking parts, semi-products or yarn scared broken end, and when weaving, Warp opening is unclear, the fabric folded phenomenon such as uneven, and what impact was produced carries out smoothly; During textiles uses, gathering of electrostatic charge easily causes dust to adhere to, and clothes tangle limbs and produce adhesion sense of discomfort; And pH value of blood can be caused to rise, in blood, in calcium content reduction, urine, calcium content increases, and blood sugar raises, Vitamin C content declines.Higher electrostatic pressure can produce electric shock to human body, and causes electronic component to damage, and even causes on fire and blast.
The preparation method of antistatic fibre forms three generations at present.First generation preparation method is at fiber surface coating surface activating agent class antistatic additive, this method is simple to operate, it is the main method that current antistatic fibre is produced, second generation preparation method refers to add surfactant-based antistatic additive or macromolecule permanent antistatic agent in the matrix polymer forming fiber, then melt spinning.The tendency of the former oriented surface migration in the fibre, can supplement impaired antistatic surface layer, be a kind of semi-permanent method; The latter and matrix polymer exist in mode that is blended or copolymerization, are formed hydrophilic " conductive channel " at fibrous inside, are a kind of permanent methods.Third generation preparation method is conductive fiber method, is to utilize carbon black, metal or metal oxide and matrix polymer to form conductive fiber.Manufacture method has adds conductive fine powder, electroless-plating and is made into finishing agent.The stable performance of conductive fiber method, excellent effect, durability is strong, and the not restriction of climate condition is the most rising method.
Antistatic acrylic fiber can be used as taking without fine hair dust-proof working of the industrial circles such as medicine, food, electronics, daily-use chemical industry, computer, precision optical machinery; Also can be used as the explosion-proof Work Clothes of oil refining, oil, smelting, coating process industry; Also can be used as the antistatics such as hospital, steamer, vehicle drapery on fire and the anti-static electricity interference such as communication, transmission of electricity fabric; Then can be used as underwear, skirt and garment lining etc. in daily life.Prepare long-acting or permanence antistatic acrylic fibers, generally adopt and in condensate, introduce hydrophilic radical to improve hygroscopicity, with a small amount of conductive materials (carbon black or metal oxide) and polyacrylonitrile matrix co-blended spinning, with copper salt solution process fiber surface, to carry out the methods such as impregnation process by conducting objects to the gel state fiber before wet spinning compacting by drying and prepare.
The antistatic method of testing of fabric commonly used by table 1
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of antistatic acrylic fiber fiber and preparation method thereof, and the inventive method is simple to operate, and parameter is easy to control, the solvent safety low toxicity used, the fibrous mechanical property of preparation is excellent, and antistatic property is good, can be applicable in anti-static fabric.
A kind of antistatic acrylic fiber fiber of the present invention, carries out wet spinning by the spinning solution containing graphene oxide, polyacrylonitrile, obtains antistatic acrylic fiber fiber; Wherein in spinning solution, the mass percentage concentration of polyacrylonitrile is 20% ~ 22%; Graphene oxide is 0.02% ~ 0.4% of polyacrylonitrile quality.
The preparation method of a kind of antistatic acrylic fiber fiber of the present invention, comprising:
The preparation method of a kind of antistatic acrylic fiber fiber of the present invention, comprising:
(1) polyacrylonitrile (PAN) dried, screen, obtain the polyacrylonitrile (PAN) after processing;
(2) by the polyacrylonitrile after above-mentioned process, graphene oxide, solvent, spinning solution is obtained;
(3) above-mentioned spinning solution is carried out vacuum filtration deaeration, wet spinning, sizing drying, obtain antistatic acrylic fiber fiber.
In described step (1), the molecular weight ranges of polyacrylonitrile (PAN) is: 60000-80000; Oven dry is: temperature-gradient method is carried out drying or constant temperature drying method; Screening is: 400 eye mesh screen screenings.
Described temperature-gradient method is dried: 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h; Constant temperature drying method is: 100 DEG C keep 6h.
In described step (2), solvent is: DMA DMAc, dimethyl sulfoxide (DMSO) DMSO, DMF DMF, sodium sulfocyanate NaSCN, acetone, ethylene carbonate EC, nitric acid HNO
3, zinc chloride ZnCl
2in one or more.Polyacrylonitrile in described step (2) after process, graphene oxide GO, solvent mode are: first add in solvent by the polyacrylonitrile (PAN) after process, and the rear heating for dissolving that expands adds graphene oxide again and forms spinning solution; Or first in solvent, add graphene oxide, add the polyacrylonitrile (PAN) heating for dissolving after process after forming dispersion again and form spinning solution; Or add PAN powder and graphene oxide simultaneously and carry out dissolving and form spinning solution; Or process after polyacrylonitrile (PAN) and graphene oxide GO be dissolved in respectively in solvent, two kinds of solution are being mixed to form spinning solution.
Graphene oxide is dissolved as: be first dissolved in the water by graphene oxide GO, then the aqueous solution is carried out frozen dried removing moisture content, then to be scattered in by GO in dicyandiamide solution or to be directly scattered in by graphene oxide GO in dicyandiamide solution and to carry out the ultrasonic process of 30 ~ 60min.
Polyacrylonitrile (PAN) after process is fully expanded in dicyandiamide solution, is specially: by the dispersion of the polyacrylonitrile (PAN) after process under the speed of agitator of 400 ~ 600 revs/min, expanded while stirring, process 2-10h.
In described step (3), wet spinning concrete technology is: in table 2.
Table 2:
The temperature that in described step (3), sizing is dry is 90-100 DEG C, and the processing time is 2-5min.
The present invention uses PAN as raw material, and based on wet spinning technology, the operation of wet spinning is: the screening of raw material is dry, prepare spinning solution, spinning solution squeezes out spinning head and forms thread, and spinning solution thread solidifies formation as-spun fibre, as-spun fibre stretching and winding, fiber post processing.
The preparation method of antistatic acrylic fiber fiber:
(1) PAN powder is dried, and screen cloth (400 order) screening is separated.
In advance PAN powder is screened, carry out filtration again after this method ratio is prepared into spinning solution and there is better effect.PAN powder feature is in table 3.
The characteristic index of table 3 polyacrylonitrile powder
| Mean molecule quantity | Range of molecular weight distributions | Vitrification point/DEG C | Density/gcm -3 | Softening Sum decomposition temperature/DEG C |
| 68000 | 60000～80000 | ≈90 | 1.12 | 220～300 |
(2) selection of spin solvent.
The solvent that can be used for PAN wet spinning has: N, N-dimethylacetylamide (DMAc), dimethyl sulfoxide (DMSO) (DMSO), DMF (DMF), sodium sulfocyanate (NaSCN), acetone, ethylene carbonate (EC), nitric acid (HNO
3) and zinc chloride (ZnCl
2) etc.Select suitable solvent according to specific needs.
(3) determination of PAN and graphene oxide content.
1. PAN mass concentration is 20% ~ 22%;
2. graphene oxide content (to PAN dry weight) is 0.02% ~ 0.4%.
(4) hybrid mode of graphene oxide, PAN powder and solvent.
Hybrid mode has four kinds, and one is first add in solvent by PAN powder, and expanded rear heating for dissolving adds graphene oxide again and forms spinning solution; Two is first in solvent, add graphene oxide, adds the expanded heating for dissolving of PAN powder again and form spinning solution after forming dispersion; Three is add PAN powder and graphene oxide to carry out dissolving and form spinning solution simultaneously; Four is that PAN and GO is dissolved in solvent respectively, and two kinds of solution are being mixed to form spinning solution; Preferred sequence is: (two) > (four) > (three) > ().
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 400 ~ 600 revs/min, expanded while stirring, process more than 2h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Contain the rotary viscosity character of GO spinning solution under using rotary viscosimeter test different temperatures, adding the viscosity influence of spinning solution of GO is little, and the viscosity of temperature to spinning solution has considerable influence, lists in table 4.During high temperature, spinning solution demonstrates low viscosity, is beneficial to the flowing of spinning solution, and during low temperature, spinning solution demonstrates low viscosity, is beneficial to spinning moulding.
The viscosity (GO4%, PAN20%) of spinning solution under table 4 different temperatures
| Temperature/DEG C | 20±1 | 30±1 | 40±1 | 50±1 | 60±1 | 70±1 |
| Viscosity/Pa.s | 84±1 | 67±1 | 56±1 | 47±1 | 33±1 | 25±1 |
(7) filter and deaeration process.
If spinning solution is even, transparent, can not filter.If containing impurity in spinning solution, according to circumstances filter with 100 ~ 200 order stainless steel meshs.
Spinning solution is transferred in the process of reactor and may has bubble generation.Therefore, after spinning solution is added reactor, need hold over night or vacuum defoamation 2h.
(8) spinning.
The spinneret orifice specification used is diameter 0.1mm × 30 circular hole, adopts three road coagulating baths to carry out spinning.With technological parameter condition listed by table 5 preferably.
The Parameter Conditions of table 5 wet spinning process process
(9) fiber drying densification and HEAT SETTING process.
By obtaining the more excellent PAN/GO fibre bundle of character to spinning fibre compacting by drying and HEAT SETTING process.Temperature 90 ~ 100 DEG C, the processing time is 2 ~ 5min.
(10) fibre property test.Mechanical property, antistatic property are all test according to national standard or industry standard.
The antistatic property surveying fiber is that the fabric adopting semi-automatic loom fiber to be made into 4.5x4.5cm size is tested.
beneficial effect
Gained fiber homogeneity of the present invention: fiber filament diameter is homogeneous, any surface finish; Mechanical property: the diameter of the average monfil of tow is 70 ± 10 μm, and TENSILE STRENGTH is 2.0 ~ 3.0cN/dtex; Along with the increase of GO amount, the brute force of fiber has rising, and when PAN concentration 20%, GO incorporation is wt%=0.02%, the average tensile fracture strength of 30 monfil is about 2.3cN/dtex, can meet the demand of weaving;
Antistatic behaviour: adopt fabric induction type static charge tester to carry out electrostatic test to fabric, frictional electrification damped method is used to measure fabric sample, when in spinning solution, GO incorporation is wt%=0.02%, when induced voltage is 10.620kV, evanescent voltage is 1.330V, and die-away time is 2.23s.
Accompanying drawing explanation
The SEM photo on the PAN/GO blended fiber surface that Fig. 1 obtains for embodiment 1.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Spinning process is:
(1) PAN powder drying and dewatering, screen cloth screening is separated.
A certain amount of PAN powder is placed in baking oven, adopts sectional heating method to dry, 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h.
400 order stainless steel mesh screen sieves are used by PAN powder after oven dry to remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of constant temperature ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMA (DMAc) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.4%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the second hybrid mode.First precision takes 0.24gGO in beaker, adds 240gDMAc, after jiggling, and ultrasonic process 15min, to dissolving fully, then accurate weighing PAN powder 60g, join in GO dispersion, after expanded 4h, be heated to 70 DEG C of dissolvings, and stir.
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 200 revs/min, expanded while stirring, process 4h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Until the dispersion of PAN powder is expanded be uniformly dispersed after, adopt thermostatical oil bath to dissolve 6h in 70 DEG C, speed of agitator is 400 revs/min, obtains the uniform spinning solution system of PAN clear.
(7) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(8) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5 parameter.
(9) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(10) spinning fibre performance test.
Prepare the advantage of fiber: as shown in Figure 1, fibre diameter is homogeneous, and surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.5cN/dtex.Table 6 demonstrates the fabric antistatic property as GOwt%=0.4%.
Embodiment 2
(1) PAN powder drying and dewatering, screen filtration is separated.Constant temperature drying method is 100 DEG C of oven dry 6h in drying box, re-use 400 order stainless steel mesh screens sieves and remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of vacuum constant temperature baking ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMA (DMAc) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.4%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the second hybrid mode.First precision takes 0.24gGO in beaker, adds 240gDMAc, after jiggling, and ultrasonic process 15min, to dissolving fully, then accurate weighing PAN powder 60g, join in GO dispersion, after expanded 4h, be heated to 70 DEG C of dissolvings, and stir.
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 200 revs/min, expanded while stirring, process 4h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Until the dispersion of PAN powder is expanded be uniformly dispersed after, adopt thermostatical oil bath to dissolve 6h in 70 DEG C, speed of agitator is 400 revs/min, obtains the uniform spinning solution system of PAN clear.
(7) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(8) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5 parameter.
(9) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(10) spinning fibre performance test.
Prepare the advantage of fiber: fibre diameter is homogeneous, surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.4cN/dtex.
Embodiment 3
Spinning process is:
(1) PAN powder drying and dewatering, screen filtration is separated.
A certain amount of PAN powder is placed in baking oven, adopts sectional heating method to dry, 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h.
400 order stainless steel mesh screen sieves are used by PAN powder after oven dry to remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of constant temperature ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMF (DMF) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.4%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the second hybrid mode.First precision takes 0.24gGO in beaker, adds 240gDMF, after jiggling, and ultrasonic process 15min, to dissolving fully, then accurate weighing PAN powder 60g, join in GO dispersion, after expanded 4h, be heated to 70 DEG C of dissolvings, and stir.
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 200 revs/min, expanded while stirring, process 4h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Until the dispersion of PAN powder is expanded be uniformly dispersed after, adopt thermostatical oil bath to dissolve 6h in 70 DEG C, speed of agitator is 400 revs/min, obtains the uniform spinning solution system of PAN clear.
(7) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(8) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5.
(9) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(10) spinning fibre performance test.
Prepare the advantage of fiber: fibre diameter is homogeneous, surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.2cN/dtex.
Embodiment 4
Spinning process is:
(1) PAN powder drying and dewatering, screen filtration is separated.
A certain amount of PAN powder is placed in baking oven, adopts sectional heating method to dry, 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h.
400 order stainless steel mesh screen sieves are used by PAN powder after oven dry to remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of constant temperature ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMA (DMAc) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.02%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the second hybrid mode.First precision takes 12mgGO in beaker, adds 240gDMAc, after jiggling, and ultrasonic process 15min, to dissolving fully, then accurate weighing PAN powder 60g, join in GO dispersion, after expanded 4h, be heated to 70 DEG C of dissolvings, and stir.
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 200 revs/min, expanded while stirring, process 4h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Until the dispersion of PAN powder is expanded be uniformly dispersed after, adopt thermostatical oil bath to dissolve 6h in 70 DEG C, speed of agitator is 400 revs/min, obtains the uniform spinning solution system of PAN clear.
(7) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(8) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5.
(9) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(10) spinning fibre performance test.
Prepare the advantage of fiber: fibre diameter is homogeneous, surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.3cN/dtex.Table 6 demonstrates, when GO content is wt%=0.02%, and the antistatic property of PAN/GO fabric.Compare with example 1, can find out, when GO content is wt%=0.02%, the antistatic property of fabric is better.
Embodiment 5
Spinning process is:
(1) PAN powder drying and dewatering, screen filtration is separated.
A certain amount of PAN powder is placed in baking oven, adopts sectional heating method to dry, 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h.
400 order stainless steel mesh screen sieves are used by PAN powder after oven dry to remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of constant temperature ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMA (DMAc) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.4%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the 4th kind of hybrid mode.Precision is taken 0.24gGO and 60gPAN to join in the beaker of 240gDMAc simultaneously, fully stir again after ultrasonic 15min.
(5) fully expanded in dicyandiamide solution of PAN powder.
By the dispersion of PAN powder under the speed of agitator of 200 revs/min, expanded while stirring, process 4h.
(6) the abundant dissolving of PAN powder in dicyandiamide solution.
Until the dispersion of PAN powder is expanded be uniformly dispersed after, adopt thermostatical oil bath to dissolve 6h in 70 DEG C, speed of agitator is 400 revs/min, obtains the uniform spinning solution system of PAN clear.
(7) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(8) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5.
(9) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(10) spinning fibre performance test.
Prepare the advantage of fiber: fibre diameter is homogeneous, surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.1cN/dtex.
Embodiment 6
Spinning process is:
(1) PAN powder drying and dewatering, screen filtration is separated.
A certain amount of PAN powder is placed in baking oven, adopts sectional heating method to dry, 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h.
400 order stainless steel mesh screen sieves are used by PAN powder after oven dry to remove bulky grain.PAN fine powder after sieve is placed in 70 DEG C of constant temperature ovens for subsequent use.
(2) selection of solvent.
Consider for volatilization rapidity, security, the easily property spun and GO dissolubility etc. are many-sided, choice for use DMA (DMAc) is as spin solvent.
(3) determination of PAN and GO content.
1. the spinning solution 300g that PAN mass concentration is 20% is prepared;
2. GO content is (to PAN mass ratio) wt%=0.4%.
(4) hybrid mode of GO, PAN and solvent.
Adopt the second hybrid mode.First precision takes 0.24gGO in beaker, adds 240gDMAc, after jiggling, and ultrasonic process 15min, to dissolving fully, then accurate weighing PAN powder 60g, join in GO dispersion.
(5) expanded, the dissolving of PAN powder in dicyandiamide solution.
The dispersion of PAN powder is placed in 70 DEG C of oil bath pans under the speed of agitator of 400 revs/min, adds thermal agitation 6h, realize expanded and dissolve, obtaining spinning solution.
(6) vacuum defoamation.
Spinning solution clear, without the need to filtering, vacuum defoamation 4h.
(7) spinning.
Three road coagulating baths are adopted to carry out spinning according to table 5.
(8) fiber drying densification and HEAT SETTING process.
At 90 DEG C of temperature, 5min is processed to spinning fibre, obtains PAN/GO fiber.
(9) spinning fibre performance test.
Prepare the advantage of fiber: fibre diameter is homogeneous, surface is comparatively bright and clean.30 monofilament average tensile fracture strengths are about 2.0cN/dtex.
The antistatic test result of the PAN/GO fabric that table 6 obtains for example 1 and example 4:
The antistatic test result of table 6PAN/GO fabric
Claims (10)
1. an antistatic acrylic fiber fiber, is characterized in that: the spinning solution containing graphene oxide, polyacrylonitrile (PAN) is carried out wet spinning, obtains antistatic acrylic fiber fiber; Wherein in spinning solution, the mass percentage concentration of polyacrylonitrile is 20% ~ 22%; Graphene oxide is 0.02% ~ 0.4% of polyacrylonitrile quality.
2. a preparation method for antistatic acrylic fiber fiber, comprising:
(1) polyacrylonitrile (PAN) dried, screen, obtain the polyacrylonitrile (PAN) after processing;
(2) by the polyacrylonitrile (PAN) after above-mentioned process, graphene oxide GO, solvent, spinning solution is obtained;
(3) above-mentioned spinning solution is carried out vacuum filtration deaeration, wet spinning, sizing drying, obtain antistatic acrylic fiber fiber.
3. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 2, is characterized in that: in described step (1), the molecular weight ranges of polyacrylonitrile (PAN) is: 60000-80000; Oven dry is: temperature-gradient method is carried out drying or constant temperature drying method; Screening is: 400 eye mesh screen screenings.
4. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 3, is characterized in that: described temperature-gradient method is dried: 60 DEG C keep 1h, are warming up to 70 DEG C, keep 1h, are warming up to 90 DEG C, keep 1h, are warming up to 120 DEG C, keep 1h; Constant temperature drying method is: 100 DEG C keep 6h.
5. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 2, it is characterized in that: the polyacrylonitrile in described step (2) after process, graphene oxide GO, solvent mode are: first add in solvent by the polyacrylonitrile (PAN) after process, the expanded rear heating for dissolving of normal temperature adds graphene oxide again and forms spinning solution; Or first in solvent, add graphene oxide, add the expanded rear heating for dissolving of the polyacrylonitrile (PAN) after process after forming dispersion again and form spinning solution; Or add PAN powder and graphene oxide simultaneously and carry out dissolving and form spinning solution; Or process after polyacrylonitrile (PAN) and graphene oxide GO be dissolved in respectively in solvent, two kinds of solution are being mixed to form spinning solution.
6. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 5, it is characterized in that: graphene oxide is dissolved as: first graphene oxide GO is dissolved in the water, again the aqueous solution is carried out frozen dried removing moisture content, then GO to be scattered in dicyandiamide solution or directly graphene oxide GO to be scattered in dicyandiamide solution and to carry out the ultrasonic process of 30 ~ 60min.
7. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 5, it is characterized in that: the polyacrylonitrile (PAN) after process is expanded, be specially: by the dispersion of the polyacrylonitrile (PAN) after process under the speed of agitator of 400 ~ 600 revs/min, expanded while stirring, process 2-10h.
8. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 2, it is characterized in that: in described step (2), solvent is: N, N-dimethylacetylamide DMAc, dimethyl sulfoxide (DMSO) DMSO, DMF DMF, sodium sulfocyanate NaSCN, acetone, ethylene carbonate EC, nitric acid HNO
3, zinc chloride ZnCl
2in one or more.
9. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 2, it is characterized in that: in described step (3), wet spinning concrete technology parameter is: coagulating bath is the mixed solution of solvent and water, temperature is 20-30 DEG C, and roller rotating speed is 2.0-3.0r/min; Elementary drawing-off bath is: pure water, temperature are 50-70 DEG C, and roller rotating speed is 3.0-4.0r/min; Hot gas spring is bathed: pure water, and temperature is 80-90 DEG C, and roller rotating speed is 8.0-15.0r/min; Winding speed is 60-70m/min.
10. the preparation method of a kind of antistatic acrylic fiber fiber according to claim 2, is characterized in that: the temperature that in described step (3), sizing is dry is 90-100 DEG C, and the processing time is 2-5min.
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Cited By (7)
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| CN106350883A (en) * | 2016-08-08 | 2017-01-25 | 青岛大学 | Preparation method of graphene oxide/polyacrylonitrile composite fiber |
| CN106958052A (en) * | 2017-04-20 | 2017-07-18 | 东华大学 | A kind of preparation method of graphene anti-static polyacrylonitrile fibre |
| CN107043960A (en) * | 2017-05-04 | 2017-08-15 | 中复神鹰碳纤维有限责任公司 | The method that a kind of useless stoste wet method of utilization polyacrylonitrile prepares functional fiber |
| CN108374208A (en) * | 2018-04-12 | 2018-08-07 | 中鸿纳米纤维技术丹阳有限公司 | A kind of dissolvant type graphene nano fiber cotton and preparation method thereof |
| CN109881286A (en) * | 2019-01-14 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | A kind of graphene flame-retardant acrylic fibre fiber and preparation method thereof |
| CN111101222A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Preparation method of graphene/polyacrylonitrile dispersion liquid |
| CN111321479A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Preparation method of graphene/polyacrylonitrile spinning solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106350883A (en) * | 2016-08-08 | 2017-01-25 | 青岛大学 | Preparation method of graphene oxide/polyacrylonitrile composite fiber |
| CN106958052A (en) * | 2017-04-20 | 2017-07-18 | 东华大学 | A kind of preparation method of graphene anti-static polyacrylonitrile fibre |
| CN106958052B (en) * | 2017-04-20 | 2019-03-01 | 东华大学 | A kind of preparation method of graphene-anti-static polyacrylonitrile fibre |
| CN107043960A (en) * | 2017-05-04 | 2017-08-15 | 中复神鹰碳纤维有限责任公司 | The method that a kind of useless stoste wet method of utilization polyacrylonitrile prepares functional fiber |
| CN108374208A (en) * | 2018-04-12 | 2018-08-07 | 中鸿纳米纤维技术丹阳有限公司 | A kind of dissolvant type graphene nano fiber cotton and preparation method thereof |
| CN111101222A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Preparation method of graphene/polyacrylonitrile dispersion liquid |
| CN111321479A (en) * | 2018-12-13 | 2020-06-23 | 中国石油化工股份有限公司 | Preparation method of graphene/polyacrylonitrile spinning solution |
| CN109881286A (en) * | 2019-01-14 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | A kind of graphene flame-retardant acrylic fibre fiber and preparation method thereof |
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