CN110437477A - A kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof - Google Patents

A kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof Download PDF

Info

Publication number
CN110437477A
CN110437477A CN201910563595.4A CN201910563595A CN110437477A CN 110437477 A CN110437477 A CN 110437477A CN 201910563595 A CN201910563595 A CN 201910563595A CN 110437477 A CN110437477 A CN 110437477A
Authority
CN
China
Prior art keywords
graphene
spinning
pet fiber
preparation
antibacterial antistatic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910563595.4A
Other languages
Chinese (zh)
Other versions
CN110437477B (en
Inventor
赵开明
王炳来
叶远丽
周永洪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Swoto Protection and Technology Co Ltd
Original Assignee
Swoto Protection and Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Swoto Protection and Technology Co Ltd filed Critical Swoto Protection and Technology Co Ltd
Priority to CN201910563595.4A priority Critical patent/CN110437477B/en
Publication of CN110437477A publication Critical patent/CN110437477A/en
Application granted granted Critical
Publication of CN110437477B publication Critical patent/CN110437477B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides

Abstract

The present invention relates to a kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof, the preparation method the following steps are included: prepare graphene dye paste, graphene dye paste and true qualities polyester slice are kneaded to be formed pigmented polyester mixture, pigmented polyester mixture melting co-extrusion, be granulated, obtain antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch.Compared with prior art, the present invention is kneaded using graphene dye paste and polyester slice, melting extrusion prepares graphene Direct-spinning of PET Fiber Masterbatch, and preparation process is stable simple controllable, and Masterbatch electrical property obtained is uniform, and antibacterial antistatic performance is durable water-fastness.

Description

A kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof
Technical field
The present invention relates to new textile materials, especially antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and its preparation side Method.
Background technique
Polyester fiber refers to that the polyester made of organic diol and binary acid or ester polycondensation synthesizes fibre through spinning is resulting Dimension, abbreviation PET fiber are the first most big chemical fibre kinds of the domestic and international volume production of current synthetic fibers.With its new function Exploitation, application field have the gesture of continuous expansion.
Graphene has highly conductive, high thermal conductivity, high-specific surface area, excellent machine as a kind of New Two Dimensional nano-carbon material The excellent characteristics such as tool performance;As a kind of super light material, the surface density of graphene is only 0.77mg/m2.Many field of textiles How graphene is compound in the textile fabrics such as polyester fiber by technical staff in research, exploitation new capability, with new application Textile material.The study found that graphene is added in polyester, the good antibacterial of polyester and antistatic effect can be assigned.But Due to the ultralight characteristic of graphene, general hybrid technique is difficult to accomplish it is compatible well with other materials.
There are mainly three types of the complex methods of current graphene and polyester fiber: first is that graphene powder is directly added in proportion Enter melt spinning in slice;Due to graphene powder large specific surface area, Ultra light-weight, although this technique be may be implemented, but very Difficulty keeps graphene evenly dispersed in the fibre.Second is that by fiber direct impregnation or padding in graphene solution, then dry, The fiber carrier of surface coated graphite alkene is obtained, can only be attached to the surface of fiber by infusion process graphene, attachment fastness is low, The graphene of attachment is often aggregating state.Third is that by the functional master batch blend spinning of polyester and containing graphene.These three sides In method, the third method graphene combines more secured in the fibre, and graphene conglomeration is less, and the more hygienic peace of production environment Entirely.
Existing graphene polyester master particle is usually used after various component powders are simply mixed in preparation and is granulated, such as Shen Please polyester master particle disclosed in the Chinese patent application number for CN109183181A be by the graphene powder that will dry etc. with gather The mixing of ester powder, granulation obtain, but the two-dimensional characteristics of graphene and nano-meter characteristic hold that graphene in polyester master particle Easy to reunite, two-dimensional characteristics are difficult to give full play to, and subsequent fiber spinning is easy broken end.Another method is such as CN109762305A Disclosed in Chinese patent application, is repeatedly padding, drying in graphene slurry, repeatedly coating using fibrous material, then making Grain;Fiber has Dagwood structure before being granulated, by repeatedly padding, wrapping up and being granulated, though graphene is improved in mother Dispersibility in grain and fiber, but the sandwich structure of heterogeneity is also inevitably introduced into master batch and subsequent fibre In dimension, and from production master batch to final finished polyester fiber, polyester material is by least wire drawing under high temperature three times, polyester property There is the deterioration that keeps away and can not exempt from.The patent application of CN108084686A also discloses a kind of conductive agglomerate of containing graphene, using stone Black alkene is mixed to form melting extrusion after dispersion liquid after the volatile organic solvent ultrasound of inertia with polyester, but there are solvents to wave The problem of environmental pollutions such as hair.In addition, there are also the methods that graphene dispersing solution is added during polycondensation of polyester, such as Patent application disclosed in CN108503804A, in contrast, this process is more complicated, needs strict control graphene dispersing solution Concentration, adding rate and polycondensation of polyester rate, if synthesis control is improper, graphene is easy to reunite, the performance of polycondensation product It is difficult to stablize guarantee.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, a kind of uniform antibacterial antistatic of performance is provided Graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof, it is intended to solve graphene and be easy in polyester master particle and polyester fiber Reunite, the problem that technical process environment is unfriendly, technique is uncontrollable.
It is an aspect of the present invention to provide a kind of preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch, institutes State preparation method the following steps are included:
S1. graphene dye paste is prepared:
S1-1, weighing and burden: formula is weighed, and formula includes: 0.5-15%S type High Temperature Disperse dye according to weight percent Material, 0.3-4% graphene oxide powder, 5-10% dispersing agent, 0.1-2% thickener, 0.05%-2% defoaming agent, remaining be Water;
S1-2. dispersion stirring: each component is put into shearing dispersator, dispersion stirs to get uniform mixture;
S1-3. nano-milled;The mixture that dispersion stirs evenly is injected ceramic nano grinder with liquid pump to carry out very Empty attrition process, reaches within 300nm to partial size, stops grinding, obtains graphene dye paste;
S2. it is kneaded;According to the weight ratio of 1:4~10, it is mixed that high speed is added in graphene dye paste and true qualities polyester slice Heating is kneaded modified coloring in mill, and melting temperature is 170-230 DEG C, forms pigmented polyester mixture;
S3. melting co-extrusion: pigmented polyester mixture through melting co-extrusion in twin (double) screw extruder, smelting temperature 190- 280 DEG C, revolving speed 120-380rpm, coloured polyester melt is processed by melt coloration;
S4. be granulated: after screw machine melting co-extrusion, tie rod, water cooling, pelletizing, drying, packaging obtain coloured polyester melt Antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch.
Graphene powder and S type High Temperature Disperse dyestuff all have phenyl ring or heterocycle structure, have good structural compatibility, The present invention mixes graphene powder and S type High Temperature Disperse dyestuff, by auxiliary agent and smooth grinding graphene powder and disperse dyes Reach that nanoscale is compatible, the graphene dye paste of stably dispersing is made;The nanoscale graphene dye paste of this liquid It is kneaded with true qualities polyester slice, melting extrusion, disperse dyes can be entered inside polyester material with either as singular molecular entities, reach molecular water Flat is compatible, and by well compatible with disperse dyes, finely dispersed graphene is also evenly into the molecule knot of polyester material In structure, promotion graphene is uniformly dispersed in polyester material well, solves graphite powder powder and disperses in polyester master particle Uneven, easy the problem of reuniting.The tinting strength, tinting power and color fastness of Masterbatch made from this process are substantially improved, coloring obtained Polyester granules can be with direct fabrics.
Preferred technical solution is that formula further includes the ethylene glycol of 0.5-3% in the step S1-1.Here, ethylene glycol It is to have good dissolution humidification to dyestuff, dispersion of the dyestuff in graphene dye paste can be promoted.
Preferred technical solution is that the dispersing agent is the compounding point for including sodium lignin sulfonate and polyvinylpyrrolidone Powder.Sodium lignin sulfonate is soluble easily in water as a kind of good surfactant, here using sodium lignin sulfonate to dyestuff Peptizaiton excellent performance, the negative electrical charge for being adsorbed in particle surface keeps particle mutually exclusive, can prevent between particle and particle Absorption, aggregation forms bulky grain and delaminating deposition disperses, grinding quality and efficiency can be promoted;It is especially mixed during the preparation process When increasing between temperature during refining, the excellent diffusivity of sodium lignin sulfonate and thermal stability make dispersion keep good Stability.Polyvinylpyrrolidone dispersing agent is a kind of high molecular surfactant, adsorbable in graphene surface, forms covering Layer, to prevent to be in contact reunion between graphene particle.It is compounded, is promoted by sodium lignin sulfonate and polyvinylpyrrolidone It is evenly dispersed in graphene dye paste into dyestuff and graphene.Preferred technical solution is matched in the step S1-1 The polyvinylpyrrolidone dispersing agent of sodium lignin sulfonate and 2-4% of the side including 3-6%.
Thickener makes graphene dye paste keep certain viscosity, prevents migration and sedimentation, promotes stability of pigment paste.It is preferred that Technical solution be, the thickener be acrylate polymer.Acrylate polymer thickener passes through carboxylic acid ion Same sex electrostatic repulsion, strand is rodlike by helical form elongation, and reticular structure is formed between disperse dyes particle, improves water Phase viscosity is to reach thickening effect.It is crucial that being dispersed with stirring with nano-grinding process slurry by lasting shear action, The thickening effect of this thickener is not influenced by shearing, guarantor of the dyestuff and graphene gradually opened by dispersion grinding by thickener Shield will not settle, therefore thickening effect is more preferable, and stability of pigment paste is higher.
Defoaming agent main function is that material is inhibited to generate bubble in the friction process of shearing dispersion.Preferred technical solution It is that the defoaming agent is non-ionic multiphase silicone polymer.Here nonionic defoaming agent, this inertia defoaming agent defoaming are used Ability is strong, and alkali resistance is strong, and good defoaming effect is especially still played in the presence of the sodium lignin sulfonate of alkalinity.
To improve dispersion effect, preferred technical solution is, in the step S1-2, first S type High Temperature Disperse dyestuff exists It is pre-dispersed in water, it is mixed in shearing dispersator after pre-dispersed with other ingredients;It is described it is pre-dispersed be to contaminate High Temperature Disperse Material is infiltrated in water, stirring and dissolving, obtains dye dispersion liquid after the filtering of 300 mesh filter screens.Graphene is improved by pre-dispersed The dispersing uniformity of dye paste.
To keep graphene dye paste performance to stablize, preferred technical solution is, pre-dispersed in the step S1-2 Water temperature is lower than 45 DEG C.Similarly, preferred technical solution further includes that in the step S1-3, the temperature control of process of lapping exists Within 50 DEG C.
To improve dispersion effect, preferred technical solution is that the step S1-3 includes rough lapping and smooth grinding two steps Suddenly.By coarse-fine grinding, grinding efficiency is improved, dyestuff and graphene is made to reach superfine nano fraction in graphene dye paste It dissipates, the tinting strength, tinting power of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch is substantially improved, can smoothly enter into following process Inside polyester material, reaches dispersion on molecular level and combine.It is further preferred that the rough lapping is 0.4mm using partial size Mill bead, the aperture 0.5mm strainer;The strainer of mill bead, the aperture 0.3mm that the smooth grinding is 0.2mm using partial size.
Another aspect of the present invention is to provide a kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch, and the antibacterial is anti- Electrostatic graphite alkene Direct-spinning of PET Fiber passes through the preparation side of above-mentioned antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch with Masterbatch Method is made.
Compared with the prior art, the advantages of the present invention are as follows the present invention is by disperse dyes, borrowing graphene dispersion Auxiliary agent and smooth grinding realization graphene are in mill base fine dispersion, between the disperse dyes after grinding carry out graphene layer, nanometer Granular disperse dyes physically act as the role for the secondary overlapping of graphene that barrier grinding is opened, and disperse dyes are protected in stone Between black alkene, graphene and dyestuff are uniformly dispersed in master batch used for spinning obtained, and Masterbatch and subsequent spinning fibre are with excellent , uniform, lasting anti-microbial property and antistatic property, stable processing performance and color fastness.Specific manifestation are as follows:
1, using graphene dye paste be kneaded with polyester slice, melting extrusion, graphene and dyestuff can smoothly into Enter in polyester material molecular structure, keep Masterbatch each component well compatible, graphene disperses more uniformly in the material, and spinning is not Easily broken end, processing energy performance are good;Due to fine dispersion, the two-dimensional characteristics of graphene are given full play to, the color fastness of dyestuff and Coloring is good;By being kneaded, water and ethylene glycol largely volatilize, and material is more closely knit, few empty after melting extrusion.
2, graphene dispersion is in S type High Temperature Disperse dyestuff, forms graphene dye paste by dispersion, by mill base with Polyester slice is kneaded, melts;Directly melt pelletization in polyester is added compared to graphene powder and prepares graphene polyester master particle, this hair Bright method purity is higher, and the content of graphene and dyestuff is easier to accurately control in Masterbatch, and the performance of Masterbatch is more stable, Industrialized production easy to accomplish.
3, the graphene dye paste mixes again with polyester slice after dispersion using water as decentralized medium, reduces graphene It disperses in the environment, the preparation process environmental pollution of Masterbatch is also less, and environmentally friendly, safety greatly improves;Due to Dyestuff color fastness and coloring in Masterbatch improve, and Masterbatch later period use process is also few to human health damage.
4, particularly the sodium lignin sulfonate and non-ionic polyvinylpyrrolidone compounding of selecting ionic point When powder, more evenly with Masterbatch performance, graphene and disperse dyes disperse antibacterial antistatic graphene Direct-spinning of PET Fiber of the present invention More evenly.
Specific embodiment
Below with reference to embodiment and comparative example, further description of the specific embodiments of the present invention.It is real in detail below The mode of applying is only used for clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1-7
A kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch is present embodiments provided, which passes through following step Suddenly it is prepared.
S1. graphene dye paste is prepared.
S1-1, weighing and burden: by S type High Temperature Disperse dyestuff include disperse red FRL 200%, disperse yellow 4RL 100%, point Dissipate black PX 300% and graphene oxide powder, ethylene glycol, dispersing agent, acrylate polymer thickener, non-ionic more Phase silicone polymer defoaming agent, water are weighed according to formula.Dispersing agent selects in sodium lignin sulfonate and polyvinylpyrrolidone It is one or two kinds of.
S1-2. dispersion stirring: disperse red FRL 200%, disperse yellow 4RL 100%, the black PX 300% of dispersion are infiltrated on In water of the temperature lower than 45 DEG C, stirring and dissolving obtains pre-dispersed dye dispersion liquid after the filtering of 300 mesh filter screens;Then dyestuff Dispersion liquid and other ingredients are added in shearing dispersator, and dispersion stirs to get uniform mixture, revolving speed 1000r/ Min, dispersion mixing time are 60min.
S1-3. nano-milled;The mixture that dispersion stirs evenly is injected ceramic nano grinder with liquid pump to carry out very Empty attrition process, grinding temperature control within 50 DEG C, and grinding process includes rough lapping and smooth grinding.Rough lapping is using partial size The strainer for grinding bead, the aperture 0.5mm of 0.4mm;The strainer of mill bead, the aperture 0.3mm that smooth grinding is 0.2mm using partial size. When 1 partial size of detection, detection partial size are reached within 300nm (d90) per hour, stops grinding, obtain the graphite of nano-dispersion Alkene dye paste.
S2. it is kneaded;According to the weight ratio of 1:4~10, it is mixed that high speed is added in graphene dye paste and true qualities polyester slice Heating is kneaded modified coloring in mill, and melting temperature is 170-230 DEG C, forms pigmented polyester mixture.
S3. melting co-extrusion: pigmented polyester mixture through melting co-extrusion in twin (double) screw extruder, smelting temperature 190- 280 DEG C, revolving speed 120-380rpm, coloured polyester melt is processed by melt coloration.
S4. be granulated: after screw machine melting co-extrusion, tie rod, water cooling, pelletizing, drying, packaging obtain coloured polyester melt Antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch.
The composition and content (weight %) that are respectively formulated in the step S1-1 of 1-7 of the embodiment of the present invention and technological parameter Selection is shown in Table 1.
Step S1-1 formula composition and embodiment technological parameter in 1 embodiment 1-7 of table
Sheet resistance test is carried out with Masterbatch to antibacterial antistatic graphene Direct-spinning of PET Fiber made from embodiment 1-7.Pressure Sheet resistance at quadrangle and centre five is tested after piece, highest sheet resistance and minimum sheet resistance are listed in table 2 respectively.It will Washing is stirred in the water added with soap lye with Masterbatch, revolving speed 600r/min washes 2h, and it is dry after washing, before test washing The antibiotic property of Masterbatch afterwards changes, and is as a result listed in table 2.By the Masterbatch spinning of antibacterial antistatic graphene Direct-spinning of PET Fiber, see Examine the processing stability in spinning process, be divided into, preferably, generally, poor four ranks;Fibrous fracture intensity after test spinning, As a result it is also found in table 2.
Comparative example 1
Unlike the first embodiment, comparative example 1 is standby using polyester slice and graphene oxide powder mixed melting co-extrusion The weight ratio of graphene polyester master particle, graphene oxide powder and polyester slice is same as Example 1, and comparative example 1 does not add S Type High Temperature Disperse dyestuff, ethylene glycol, water, non-ionic multiphase silicone polymer defoaming agent, acrylate polymer thickener, wood Quality sodium sulfonate, polyvinylpyrrolidone.Equally test and have evaluated the surface electricity for the graphene polyester master particle that comparative example 1 obtains Fibrous fracture intensity after resistance, antibiotic property, the processing stability of spinning process, spinning, the results are shown in Table 2.
Comparative example 2
Unlike the first embodiment, comparative example 2 is standby using polyester slice and graphene oxide powder mixed melting co-extrusion The weight ratio of graphene polyester master particle, graphene oxide powder and polyester slice is same as Example 1.Comparative example 2 does not add S Type High Temperature Disperse dyestuff, ethylene glycol, water, non-ionic multiphase silicone polymer defoaming agent, acrylate polymer thickener, add Added graphene oxide powder, sodium lignin sulfonate, polyvinylpyrrolidone, this three respectively with the weight ratio of polyester slice with Embodiment 1 is identical.The sheet resistance and processing for equally testing and having evaluated the graphene polyester master particle that comparative example 2 obtains are stablized Property, it the results are shown in Table 2.
The Masterbatch of 2 embodiment 1-7 of table preparation and the master batch the performance test results of comparative example 1-2 preparation
As seen from the results in Table 2, melting extrusion is granulated after graphene oxide powder and polyester slice are simply mixed, and is obtained Master batch resistance fluctuation reach the 2-3 order of magnitude.And the antibacterial antistatic graphene polyester as made from embodiment 1-7 method is spun Silk in an order of magnitude, fluctuates minimum with Masterbatch resistance fluctuation, and antibacterial effect is more preferably more longlasting water-fastness, and when spinning adds Apt qualitative more preferable, fibre strength is higher.
In addition, can be seen that addition of the ethylene glycol in graphene dye paste from embodiment 1 and embodiment 5-7, and It is compounded by sodium lignin sulfonate and polyvinylpyrrolidone, more evenly, antibiotic property is more longlasting for Masterbatch electric conductivity obtained It is water-fastness;The breaking strength of spinning fibre is higher, processes more stable.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch, which is characterized in that the preparation method The following steps are included:
S1. graphene dye paste is prepared:
S1-1, weighing and burden: will formula weighing, formula according to weight percent include: 0.5-15%S type High Temperature Disperse dyestuff, 0.3-4% graphene oxide powder, 5-10% dispersing agent, 0.1-2% thickener, 0.05%-2% defoaming agent, remaining be water;
S1-2. dispersion stirring: each component is put into shearing dispersator, dispersion stirs to get uniform mixture;
S1-3. nano-milled;The mixture injection ceramic nano grinder that dispersion is stirred evenly carries out vacuum attrition process, to Partial size reaches within 300nm, stops grinding, obtains graphene dye paste;
S2. it is kneaded;According to the weight ratio of 1:4~10, high speed mixing smelting machine is added in graphene dye paste and true qualities polyester slice Interior heating is kneaded modified coloring, and melting temperature is 170-230 DEG C, forms pigmented polyester mixture;
S3. melting co-extrusion: pigmented polyester mixture through melting co-extrusion in twin (double) screw extruder, smelting temperature is 190-280 DEG C, Revolving speed is 120-380rpm, is processed into coloured polyester melt by melt coloration;
S4. be granulated: for coloured polyester melt after screw machine melting co-extrusion, tie rod, water cooling, pelletizing, drying, packaging obtain antibacterial Antistatic graphene Direct-spinning of PET Fiber Masterbatch.
2. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that Formula further includes the ethylene glycol of 0.5-3% in the step S1-1.
3. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that The dispersing agent is the compounding dispersing agent for including sodium lignin sulfonate and polyvinylpyrrolidone.
4. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that The thickener is acrylate polymer.
5. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that The defoaming agent is non-ionic multiphase silicone polymer.
6. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that First that High Temperature Disperse dyestuff is pre-dispersed in water in the step S1-2, after pre-dispersed and other ingredients are in shearing dispersion stirring It is mixed in machine;It is described it is pre-dispersed be S type High Temperature Disperse dyestuff to be infiltrated in water, stirring and dissolving, through 300 mesh filter screens filtering after Obtain dye dispersion liquid.
7. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as claimed in claim 6, which is characterized in that In the step S1-2, pre-dispersed water temperature is lower than 45 DEG C.
8. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as described in claim 1, which is characterized in that In the step S1-3, the temperature of process of lapping is controlled within 50 DEG C.
9. the preparation method of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch as claimed in claim 8, it is characterised in that; The step S1-3 includes two steps of rough lapping and smooth grinding;The rough lapping using partial size be 0.4mm mill bead, The strainer in the aperture 0.5mm, the strainer of mill bead, the aperture 0.3mm that the smooth grinding is 0.2mm using partial size.
10. a kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch, which is characterized in that the antibacterial antistatic graphene is poly- Ester master batch used for spinning passes through antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch described in any one of claim 1-9 Preparation method is made.
CN201910563595.4A 2019-06-26 2019-06-26 Antibacterial antistatic graphene polyester spinning color master batch and preparation method thereof Active CN110437477B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910563595.4A CN110437477B (en) 2019-06-26 2019-06-26 Antibacterial antistatic graphene polyester spinning color master batch and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910563595.4A CN110437477B (en) 2019-06-26 2019-06-26 Antibacterial antistatic graphene polyester spinning color master batch and preparation method thereof

Publications (2)

Publication Number Publication Date
CN110437477A true CN110437477A (en) 2019-11-12
CN110437477B CN110437477B (en) 2022-03-15

Family

ID=68429040

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910563595.4A Active CN110437477B (en) 2019-06-26 2019-06-26 Antibacterial antistatic graphene polyester spinning color master batch and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110437477B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110952155A (en) * 2019-11-20 2020-04-03 浙江佳人新材料有限公司 Production process of cyclic regeneration antistatic fiber
CN111254537A (en) * 2019-12-19 2020-06-09 浙江麻尚生纺织科技有限公司 Fiber fabric and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140048738A1 (en) * 2010-12-28 2014-02-20 Shanghai Genius Advanced Material(Group) Co., Ltd. Nano particle/polyamide composite material, preparation method therefor, and use thereof
CN103710790A (en) * 2013-12-30 2014-04-09 厦门翔鹭化纤股份有限公司 Antistatic, antibacterial and graphene-reinforced composite polyester fiber and preparation method thereof
CN105200547A (en) * 2015-10-19 2015-12-30 沙嫣 Preparation method of graphene-polyester nano-composite fiber
CN107189412A (en) * 2017-06-13 2017-09-22 浙江金彩新材料有限公司 It is a kind of for graphene heat discoloration Masterbatch of Fypro and preparation method thereof
CN107501714A (en) * 2017-09-01 2017-12-22 金发科技股份有限公司 A kind of polypropene composition and preparation method thereof
CN108102313A (en) * 2018-01-16 2018-06-01 苏州市苏宏塑料有限公司 A kind of dyeing polyester master batch and its production technology
CN108864561A (en) * 2017-05-08 2018-11-23 山东圣泉新材料股份有限公司 A kind of modified master batch, modified fibre prepared therefrom, modification nonwoven cloth and its preparation method and application

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140048738A1 (en) * 2010-12-28 2014-02-20 Shanghai Genius Advanced Material(Group) Co., Ltd. Nano particle/polyamide composite material, preparation method therefor, and use thereof
CN103710790A (en) * 2013-12-30 2014-04-09 厦门翔鹭化纤股份有限公司 Antistatic, antibacterial and graphene-reinforced composite polyester fiber and preparation method thereof
CN105200547A (en) * 2015-10-19 2015-12-30 沙嫣 Preparation method of graphene-polyester nano-composite fiber
CN108864561A (en) * 2017-05-08 2018-11-23 山东圣泉新材料股份有限公司 A kind of modified master batch, modified fibre prepared therefrom, modification nonwoven cloth and its preparation method and application
CN107189412A (en) * 2017-06-13 2017-09-22 浙江金彩新材料有限公司 It is a kind of for graphene heat discoloration Masterbatch of Fypro and preparation method thereof
CN107501714A (en) * 2017-09-01 2017-12-22 金发科技股份有限公司 A kind of polypropene composition and preparation method thereof
CN108102313A (en) * 2018-01-16 2018-06-01 苏州市苏宏塑料有限公司 A kind of dyeing polyester master batch and its production technology

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王双成等: "石墨烯改性锦纶6母粒制备及性能分析", 《山东纺织科技》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110952155A (en) * 2019-11-20 2020-04-03 浙江佳人新材料有限公司 Production process of cyclic regeneration antistatic fiber
CN111254537A (en) * 2019-12-19 2020-06-09 浙江麻尚生纺织科技有限公司 Fiber fabric and preparation method thereof

Also Published As

Publication number Publication date
CN110437477B (en) 2022-03-15

Similar Documents

Publication Publication Date Title
CN110437477A (en) A kind of antibacterial antistatic graphene Direct-spinning of PET Fiber Masterbatch and preparation method thereof
CN104884687B (en) The preparation method of Multifunctional polyester fiber and the Multifunctional polyester fiber thus prepared
MX2007008404A (en) Slurries containing microfiber and micropowder, and methods for using and making same.
CN103752848B (en) A kind of preparation method of nano-silver thread
US20210130986A1 (en) Plant-based functional polyester filament and preparation method thereof
CN104059275B (en) A kind of diatomite substitutes polyolefin color masterbatch of part pigment and preparation method thereof
CN101392077A (en) Polypropylene color master-batch with pearlescent interference effect and preparation method thereof
CN107418159B (en) BOPET ultraviolet screener master batch and its manufacturing method
CN110437479A (en) A kind of antibacterial antistatic graphene polypropylene spinning Masterbatch and preparation method thereof
CN102953148B (en) Low-melting-point polyester skin core composite colored fiber and production method thereof
CN101085845A (en) Conducting fibre master batch and preparation method thereof
CN109137128A (en) A kind of anion terylene fiber and preparation method thereof
CN108866672A (en) A method of improving polyester fiber vividness and tinting strength, tinting power
CN110437478A (en) A kind of antibacterial antistatic graphene extrusion spinning Masterbatch and preparation method thereof
CN109401218A (en) A kind of heat discoloration Masterbatch and preparation method for polyester fiber
CN108690336B (en) Biodegradable polylactic acid agricultural mulching film and processing technology thereof
CN109706534A (en) A kind of ultra high molecular weight polyethylene fiber color oil and preparation method thereof
CN110367610A (en) A kind of antibacterial deodourizing socks and its manufacturing method
CN108193316A (en) A kind of original liquid coloring acid fiber by polylactic and preparation method thereof
CN106751582A (en) A kind of polyester polyethylene bicomponent fibers color concentrate and preparation method thereof
CN111363346A (en) Method for preparing antistatic black master batch by using graphene coated carbon black and product
CN110004508A (en) A kind of melt spun spandex Masterbatch and preparation method thereof
CN203794818U (en) Production system for continuous production of direct-spinning copolymer type antistatic polyester
CN103012943A (en) Method for preparing high-solute LDPE (Low-Density Polyethylene) powder dispersant color masterbatch
CN102877154B (en) Method for preparing organic pigment microcapsule polyester color yarn

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant