CN109267348A - A kind of preparation method and applications of the textile material added with graphene - Google Patents
A kind of preparation method and applications of the textile material added with graphene Download PDFInfo
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- CN109267348A CN109267348A CN201811014433.7A CN201811014433A CN109267348A CN 109267348 A CN109267348 A CN 109267348A CN 201811014433 A CN201811014433 A CN 201811014433A CN 109267348 A CN109267348 A CN 109267348A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation method and applications of textile material added with graphene, this method is used acid fiber by polylactic, doughnut is immersed in NaOH solution and is ultrasonically treated, it is transferred in autoclave after then the sediment being centrifugated out is washed with deionized to neutrality, melamine resin is added to be stirred to react at high temperature under high pressure, the reaction under high pressure product and Repudin-Special that will be obtained again, zinc ricinate, graphene oxide, it is granulated after crosslinking agent mixing through melt extruded and fiber grain is made, obtained fiber grain is obtained into fiber filaments through melt spinning, using stretching, sizing, weaving handles to obtain fabric, then pre-process fabric is modified, digestion, add finishing agent, continue digestion, cloth outputting, dehydration, drying obtains finished product textile material.The textile material being prepared has preferable fungistatic effect, has a good application prospect in medical Clothing Industry.
Description
Technical field
The present invention relates to textile material technical fields, and in particular to a kind of preparation side of the textile material added with graphene
Method and its application.
Background technique
Textile in the prior art is generally made of materials such as cotton fiber or polyester fibers, does not have bacteria resistance function, respectively
Class harmful bacteria promotes the diffusion sprawling of pandemic by the propagation of textile product.Antibacterial textile material has good peace
Quan Xing, it can efficiently completely remove bacterium, fungi and mould on fabric, keep clean fabric, and can prevent bacteriological aftergrowth
And breeding.Much antibacterial means used are mostly used to be added into textile is reported to the research of the antibacterial processing of textile material at present
Add bacteriostatic agent such as quaternary ammonium salt, guanidine, fatty acid and metallic compound etc., wherein bacteriostatic agent itself has toxicity, not ring
It protects, some bacteriostatic agents are at high cost, processing technology is complicated, and in addition to this it is difficult often to have antibacterial drug effect for existing antibacterial class textile
With maintenance, bio-refractory, pollutes environment, is unfavorable for the disadvantages of environmental-friendly.
Summary of the invention
Based on current textile material the problem of bacteriostasis property is not still able to satisfy consumer demand, the present invention provides one kind and adds
Added with the preparation method and applications of the textile material of graphene.
A kind of preparation method of the textile material added with graphene, comprising the following steps:
(1) by 75-85 parts of acid fiber by polylactic, 8-10 parts of doughnut be immersed in concentration be 5mol/L NaOH solution in into
Row ultrasonic treatment, then will ultrasonic treatment mixed liquor by being centrifugated out sediment, by sediment be washed with deionized to
It is transferred in autoclave after neutrality, is added melamine resin 6-8 parts, is stirred to react at high temperature under high pressure, obtains reaction under high pressure
Product；
(2) the reaction under high pressure product for obtaining step (1) with Repudin-Special 4-6 parts, 3-5 parts of zinc ricinate,
In 3-5 parts of graphene oxide, 1-3 parts of crosslinking agent common addition high-speed mixers, carried out with 1000-1200 revs/min of rate
It is stirred, then puts into mixed material in double screw extruder, be granulated through melt extruded and fiber grain is made；
(3) fiber grain that step (2) obtains is added in melt spinning machine, by each area's temperature of melt spinning machine point
Fiber filaments Kong Zhi not be obtained through melt spinning in 135-145 DEG C, 150-160 DEG C, 175-185 DEG C, 175-195 DEG C, using
Stretching, sizing, weaving handle to obtain fabric, and draw ratio is 3-5 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and hot water storgae water temperature is 80-
90 DEG C, holding time is 30-40 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, stirs at low speed 2- at room temperature
3 hours, stirring rate was 80-100 revs/min, then pulls modified fabric out, washs 2-3 with the ethanol water of 90wt%
It is secondary, then be washed with deionized 1-2 times, then the modification fabric after washing is immersed in the hot water storgae of desizing, scouring and bleaching combined machine, if
Determining bath raio is 1:25, is first cleaned 30-40 minutes, then cleaned 15-20 minutes with 90-95 DEG C of water, is obtained pre- with 75-85 DEG C of water
Handle modified fabric；
(6) the deionized water digestion 100-120 that the pretreatment modification fabric for obtaining step (5) is 80-90 DEG C with temperature
Minute, finishing agent is added, is continued digestion 40-50 minutes, cloth outputting, dehydration, drying obtain finished product textile material.
Preparation is participated in present invention employs Repudin-Special, zinc ricinate, graphene oxide these types raw material to spin
Material is knitted, effective performance improvement has been carried out to textile material, although these materials are not applied in textile material for the first time,
Amount group merges and in advance producing reaction under high pressure made of acid fiber by polylactic, doughnut and melamine resin according to a certain ratio
Fiber grain is made in object jointly, brings the improvement in service performance to the textile material being finally prepared, this is previous
It is never to report in research, for realizing that it is conclusive that technical effect of the invention plays the role of.
Further, the frequency being ultrasonically treated in the step (1) is 22-24kHz, power 220-250W, when processing
Between be 15-20 minutes.
Further, the specific ginseng being stirred to react at high temperature under high pressure in autoclave in the step (1)
Number are as follows: pressure 10-12MPa, temperature are 120-140 DEG C, stirring rate is 220-240 revs/min, reaction time 15-25
Minute.
Further, which is characterized in that the screw speed of double screw extruder is 250 revs/min in the step (2),
Head temperature is 80-85 DEG C.
Further, the modifying agent in the step (4) is sodium sulfate of polyethenoxy ether of fatty alcohol, diethylene glycol, chlorination
Polyethylene according to 2:3:6 mass ratio composed by mixture.
Further, the concentration of finishing agent in water is 1wt% in the step (6).
The invention also discloses the textile material of graphene is added with made from above-mentioned preparation method in medical Clothing Industry
In application.
The textile material that preparation method through the invention is prepared has preferable fungistatic effect, in medical dress ornament
It has a good application prospect in industry.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below in conjunction with specific embodiment,
The present invention will be described in further detail.It should be appreciated that the specific embodiments described herein are only used to explain this hair
It is bright, it is not intended to limit the present invention.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more
Any and all combinations of relevant listed item.
Raw materials used and reagent is commercially available common raw material and reagent in following embodiment.
A kind of preparation method of the textile material added with graphene, comprising the following steps:
(1) by 75-85 parts of acid fiber by polylactic, 8-10 parts of doughnut be immersed in concentration be 5mol/L NaOH solution in into
Row ultrasonic treatment, then will ultrasonic treatment mixed liquor by being centrifugated out sediment, by sediment be washed with deionized to
It is transferred in autoclave after neutrality, is added melamine resin 6-8 parts, is stirred to react at high temperature under high pressure, obtains reaction under high pressure
Product；
(2) the reaction under high pressure product for obtaining step (1) with Repudin-Special 4-6 parts, 3-5 parts of zinc ricinate,
In 3-5 parts of graphene oxide, 1-3 parts of crosslinking agent common addition high-speed mixers, carried out with 1000-1200 revs/min of rate
It is stirred, then puts into mixed material in double screw extruder, be granulated through melt extruded and fiber grain is made；
(3) fiber grain that step (2) obtains is added in melt spinning machine, by each area's temperature of melt spinning machine point
Fiber filaments Kong Zhi not be obtained through melt spinning in 135-145 DEG C, 150-160 DEG C, 175-185 DEG C, 175-195 DEG C, using
Stretching, sizing, weaving handle to obtain fabric, and draw ratio is 3-5 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and hot water storgae water temperature is 80-
90 DEG C, holding time is 30-40 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, stirs at low speed 2- at room temperature
3 hours, stirring rate was 80-100 revs/min, then pulls modified fabric out, washs 2-3 with the ethanol water of 90wt%
It is secondary, then be washed with deionized 1-2 times, then the modification fabric after washing is immersed in the hot water storgae of desizing, scouring and bleaching combined machine, if
Determining bath raio is 1:25, is first cleaned 30-40 minutes, then cleaned 15-20 minutes with 90-95 DEG C of water, is obtained pre- with 75-85 DEG C of water
Handle modified fabric；
(6) the deionized water digestion 100-120 that the pretreatment modification fabric for obtaining step (5) is 80-90 DEG C with temperature
Minute, finishing agent is added, is continued digestion 40-50 minutes, cloth outputting, dehydration, drying obtain finished product textile material.
Wherein, amount group merges and leads in advance according to a certain ratio for Repudin-Special, zinc ricinate, graphene oxide
It crosses and fiber grain has been made in reaction under high pressure product made of acid fiber by polylactic, doughnut and melamine resin jointly.It compares
It is of the invention that changing for matter has occurred on the molecular structure of fiber grain for fiber grain only is made by reaction under high pressure product
Become, this is because cross-linking reaction has occurred with the fibre composition in reaction under high pressure product at a certain temperature in above compound,
The higher structure of more high-order is formd, so that the textile material being finally prepared be made to be not easy the attachment as bacterial reproduction
Face realizes fungistatic effect.
In a preferred embodiment, the frequency being ultrasonically treated in the step (1) is 22-24kHz, power 220-
250W, processing time are 15-20 minutes.
In a preferred embodiment, it is stirred at high temperature under high pressure in autoclave in the step (1)
The design parameter of reaction are as follows: pressure 10-12MPa, temperature are 120-140 DEG C, stirring rate is 220-240 revs/min, reaction
Time is 15-25 minutes.
In a preferred embodiment, the screw speed of double screw extruder is 250 revs/min in the step (2),
Head temperature is 80-85 DEG C.
In a preferred embodiment, the modifying agent in the step (4) is sodium sulfate of polyethenoxy ether of fatty alcohol, two
Ethylene glycol, haloflex according to 2:3:6 mass ratio composed by mixture.
In a preferred embodiment, the concentration of finishing agent in water is 1wt% in the step (6).
Present invention also provides the textile material of graphene is added with made from the preparation method in medical Clothing Industry
In application.
Below by embodiment, the present invention is furture elucidated.It should be pointed out that the present invention is not intended to be limited to the reality
Apply example.
Embodiment 1
(1) 75 parts of acid fiber by polylactic, 8 parts of doughnut are immersed in the NaOH solution that concentration is 5mol/L and carry out ultrasound
Processing, the frequency of ultrasonic treatment are 22kHz, power 220W, and the processing time is 15 minutes, then lead to ultrasonic treatment mixed liquor
It crosses and is centrifugated out sediment, be transferred to after sediment is washed with deionized to neutrality in autoclave, melamine is added
6 parts of resin, set the pressure of autoclave as 10MPa, temperature be 120 DEG C, stirring rate is 220 revs/min, react 15 points
Clock obtains reaction under high pressure product；
(2) the reaction under high pressure product for obtaining step (1) and 4 parts of Repudin-Special, 3 parts of zinc ricinate, oxidation
In 3 parts of graphene, 1 part of crosslinking agent common addition high-speed mixer, mixing is stirred with 1000 revs/min of rate, then
Mixed material is put into double screw extruder, sets screw speed as 250 revs/min, head temperature is 80 DEG C, is squeezed through melting
Pressure, which is granulated, is made fiber grain；
(3) fiber grain that step (2) obtains is added in melt spinning machine, by each area's temperature of melt spinning machine point
Fiber filaments Kong Zhi not be obtained through melt spinning, at stretching, sizing, weaving in 135 DEG C, 150 DEG C, 175 DEG C, 175 DEG C
Reason obtains fabric, and draw ratio is 3 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and modifying agent is fatty alcohol
Polyethenoxy ether sodium sulfate, diethylene glycol, haloflex according to 2:3:6 mass ratio composed by mixture, hot water storgae
Water temperature is 80 DEG C, and holding time is 30 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, stirs at low speed 2 at room temperature
Hour, stirring rate is 80 revs/min, then modified fabric pulled out, is washed 2-3 times with the ethanol water of 90wt%, then
It is washed with deionized 1-2 times, then immerses the modification fabric after washing in the hot water storgae of desizing, scouring and bleaching combined machine, set bath raio
It for 1:25, is first cleaned 30 minutes with 75 DEG C of water, then is cleaned 15 minutes with 90 DEG C of water, obtain pretreatment modification fabric；
(6) the pretreatment modification fabric temperature for obtaining step (5) is deionized water digestion 100 minutes of 80 DEG C, then
Finishing agent is added, the concentration of finishing agent in water is 1wt%, is continued digestion 40 minutes, and cloth outputting, dehydration, drying obtain finished product spinning
Knit material.
Embodiment 2
(1) 80 parts of acid fiber by polylactic, 9 parts of doughnut are immersed in the NaOH solution that concentration is 5mol/L and carry out ultrasound
Processing, the frequency of ultrasonic treatment are 23kHz, power 235W, and the processing time is 18 minutes, then lead to ultrasonic treatment mixed liquor
It crosses and is centrifugated out sediment, be transferred to after sediment is washed with deionized to neutrality in autoclave, melamine is added
7 parts of resin, set the pressure of autoclave as 11MPa, temperature be 130 DEG C, stirring rate is 230 revs/min, react 20 points
Clock obtains reaction under high pressure product；
(2) the reaction under high pressure product for obtaining step (1) and 5 parts of Repudin-Special, 4 parts of zinc ricinate, oxidation
In 4 parts of graphene, 2 parts of crosslinking agent common addition high-speed mixers, mixing is stirred with 1100 revs/min of rate, then
Mixed material is put into double screw extruder, sets screw speed as 250 revs/min, head temperature is 82.5 DEG C, through melting
Fiber grain is made in extrusion granulation；
(3) fiber grain that step (2) obtains is added in melt spinning machine, by each area's temperature of melt spinning machine point
Fiber filaments Kong Zhi not be obtained through melt spinning, at stretching, sizing, weaving in 140 DEG C, 155 DEG C, 180 DEG C, 185 DEG C
Reason obtains fabric, and draw ratio is 4 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and modifying agent is fatty alcohol
Polyethenoxy ether sodium sulfate, diethylene glycol, haloflex according to 2:3:6 mass ratio composed by mixture, hot water storgae
Water temperature is 85 DEG C, and holding time is 35 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, stirs at low speed at room temperature
2.5 hours, stirring rate was 90 revs/min, then pulls modified fabric out, is washed 2-3 times with the ethanol water of 90wt%,
It is washed with deionized 1-2 times, then immerses the modification fabric after washing in the hot water storgae of desizing, scouring and bleaching combined machine again, setting bath
It than first being cleaned 35 minutes with 80 DEG C of water for 1:25, then is cleaned 18 minutes with 93 DEG C of water, obtains pretreatment modification fabric；
(6) the pretreatment modification fabric temperature for obtaining step (5) is deionized water digestion 110 minutes of 85 DEG C, then
Finishing agent is added, the concentration of finishing agent in water is 1wt%, is continued digestion 45 minutes, and cloth outputting, dehydration, drying obtain finished product spinning
Knit material.
Embodiment 3
(1) 85 parts of acid fiber by polylactic, 10 parts of doughnut are immersed in the NaOH solution that concentration is 5mol/L and are surpassed
Sonication, the frequency of ultrasonic treatment are 24kHz, power 250W, and the processing time is 20 minutes, will then be ultrasonically treated mixed liquor
It by being centrifugated out sediment, is transferred to after sediment is washed with deionized to neutrality in autoclave, honey is added
8 parts of polyimide resin, set the pressure of autoclave as 12MPa, temperature be 140 DEG C, stirring rate is 240 revs/min, reaction 25
Minute, obtain reaction under high pressure product；
(2) the reaction under high pressure product for obtaining step (1) and 6 parts of Repudin-Special, 5 parts of zinc ricinate, oxidation
In 5 parts of graphene, 3 parts of crosslinking agent common addition high-speed mixers, mixing is stirred with 1200 revs/min of rate, then
Mixed material is put into double screw extruder, sets screw speed as 250 revs/min, head temperature is 85 DEG C, is squeezed through melting
Pressure, which is granulated, is made fiber grain；
(3) fiber grain that step (2) obtains is added in melt spinning machine, by each area's temperature of melt spinning machine point
Fiber filaments Kong Zhi not be obtained through melt spinning, at stretching, sizing, weaving in 145 DEG C, 160 DEG C, 185 DEG C, 195 DEG C
Reason obtains fabric, and draw ratio is 5 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and modifying agent is fatty alcohol
Polyethenoxy ether sodium sulfate, diethylene glycol, haloflex according to 2:3:6 mass ratio composed by mixture, hot water storgae
Water temperature is 90 DEG C, and holding time is 40 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, stirs at low speed 3 at room temperature
Hour, stirring rate is 100 revs/min, then modified fabric pulled out, is washed 2-3 times with the ethanol water of 90wt%, then
It is washed with deionized 1-2 times, then immerses the modification fabric after washing in the hot water storgae of desizing, scouring and bleaching combined machine, set bath raio
It for 1:25, is first cleaned 40 minutes with 85 DEG C of water, then is cleaned 20 minutes with 95 DEG C of water, obtain pretreatment modification fabric；
(6) the pretreatment modification fabric for obtaining step (5) is with deionized water digestion at a temperature of 90 °C 120 minutes, then
Finishing agent is added, the concentration of finishing agent in water is 1wt%, is continued digestion 50 minutes, and cloth outputting, dehydration, drying obtain finished product spinning
Knit material.
Comparative example 1
Raw material used in the textile material of this comparative example and preparation method are substantially with embodiment 1, and difference is, in step
(2) in the mixed process in, Repudin-Special is not added.
Comparative example 2
Raw material used in the textile material of this comparative example and preparation method are substantially with embodiment 1, and difference is, in step
(2) in the mixed process in, zinc ricinate is not added.
Comparative example 3
Raw material used in the textile material of this comparative example and preparation method are substantially with embodiment 1, and difference is, in step
(2) in the mixed process in, graphene oxide is not added.
Comparative example 4
Raw material used in the textile material of this comparative example and preparation method are substantially with embodiment 1, and difference is, in step
(2) Screw Extrusion granulation is carried out after directly mixing reaction under high pressure product with crosslinking agent in.
Performance test
Test method according to national standards carries out textile material prepared by embodiment 1-3 and comparative example 1-4
Bacteriostasis property test.
Table 1
| Escherichia coli bacteriostasis rate (%) | Staphylococcus aureus bacteriostasis rate (%) | |
| Embodiment 1 | 96 | 94 |
| Embodiment 2 | 97 | 95 |
| Embodiment 3 | 95 | 94 |
| Comparative example 1 | 82 | 81 |
| Comparative example 2 | 84 | 82 |
| Comparative example 3 | 79 | 76 |
| Comparative example 4 | 67 | 63 |
Test result is as shown above, and the textile material of embodiment 1-3 is pressing down compared with the textile material of comparative example 1-4
It is more significant in bacterium effect.Illustrate textile material of the present invention it is raw materials used in Repudin-Special, zinc ricinate, oxidation
There is the facilitation for improving and existing on textile material bacteriostasis property and mutually cooperateing between graphene.
To sum up, the preparation method of textile material of the invention is used acid fiber by polylactic, that doughnut is immersed in NaOH is molten
It is ultrasonically treated in liquid, is transferred to reaction under high pressure after then the sediment being centrifugated out is washed with deionized to neutrality
In kettle, melamine resin is added and is stirred to react at high temperature under high pressure, then by obtained reaction under high pressure product and Repudin-Special,
It is granulated after zinc ricinate, graphene oxide, crosslinking agent mixing through melt extruded and fiber grain, the fiber grain that will be obtained is made
Fiber filaments are obtained through melt spinning, handle to obtain fabric using stretching, sizing, weaving, then by the modified progress of fabric
Pretreatment, digestion add finishing agent, continue digestion, cloth outputting, dehydration, drying obtain finished product textile material.The spinning being prepared
Material is knitted, has preferable fungistatic effect, is had a good application prospect in medical Clothing Industry.Also, the present invention uses
Repudin-Special, zinc ricinate, graphene oxide these types raw material participation prepare textile material, to textile material into
Effective performance improvement of having gone is measured according to a certain ratio and is combined although these materials are not applied in textile material for the first time
And in advance by the way that fiber is made in reaction under high pressure product made of acid fiber by polylactic, doughnut and melamine resin jointly
Grain, brings the improvement in service performance to the textile material being finally prepared, this is never to report in previous research
It crosses, for realizing that it is conclusive that technical effect of the invention plays the role of.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.
Claims (7)
1. a kind of preparation method of the textile material added with graphene, which comprises the following steps:
(1) 75-85 parts of acid fiber by polylactic, 8-10 parts of doughnut are immersed in the NaOH solution that concentration is 5mol/L and are surpassed
Then sediment is washed with deionized to neutrality by being centrifugated out sediment for ultrasonic treatment mixed liquor for sonication
After be transferred in autoclave, be added melamine resin 6-8 parts, be stirred to react at high temperature under high pressure, obtain reaction under high pressure product；
(2) the reaction under high pressure product for obtaining step (1) and Repudin-Special 4-6 parts, 3-5 parts of zinc ricinate, oxidation
In 3-5 parts of graphene, 1-3 parts of crosslinking agent common addition high-speed mixers, it is stirred with 1000-1200 revs/min of rate
Mixing then puts into mixed material in double screw extruder, is granulated through melt extruded and fiber grain is made；
(3) fiber grain that step (2) obtains is added in melt spinning machine, each area's temperature of melt spinning machine is controlled respectively
System obtains fiber filaments through melt spinning, using drawing in 135-145 DEG C, 150-160 DEG C, 175-185 DEG C, 175-195 DEG C
Stretch, be formed, weaving handles to obtain fabric, draw ratio is 3-5 times；
(4) fabric for obtaining step (3) immerses in the hot water storgae containing 0.5wt% modifying agent, and hot water storgae water temperature is 80-90
DEG C, holding time is 30-40 minutes, obtains modified fabric；
(5) the modification fabric for obtaining step (4) immerses in the ethanol water of 75wt%, and it is small to stir at low speed 2-3 at room temperature
When, stirring rate is 80-100 revs/min, then modified fabric pulled out, is washed 2-3 times with the ethanol water of 90wt%,
It is washed with deionized 1-2 times, then immerses the modification fabric after washing in the hot water storgae of desizing, scouring and bleaching combined machine again, setting bath
It than first being cleaned 30-40 minutes with 75-85 DEG C of water for 1:25, then is cleaned 15-20 minutes, is pre-processed with 90-95 DEG C of water
Modified fabric；
(6) the pretreatment modification fabric for obtaining step (5) be 80-90 DEG C with temperature deionized water digestion 100-120 minutes,
Finishing agent is added, is continued digestion 40-50 minutes, cloth outputting, dehydration, drying obtain finished product textile material.
2. the preparation method of the textile material according to claim 1 added with graphene, which is characterized in that the step
(1) frequency being ultrasonically treated in is 22-24kHz, power 220-250W, and the processing time is 15-20 minutes.
3. the preparation method of the textile material according to claim 1 added with graphene, which is characterized in that the step
(1) design parameter being stirred to react at high temperature under high pressure in autoclave in are as follows: pressure 10-12MPa, temperature are
120-140 DEG C, stirring rate be 220-240 revs/min, the reaction time be 15-25 minutes.
4. the preparation method of the textile material according to claim 1 added with graphene, which is characterized in that the step
(2) screw speed of double screw extruder is 250 revs/min in, and head temperature is 80-85 DEG C.
5. the preparation method of the textile material according to claim 1 added with graphene, which is characterized in that the step
(4) modifying agent in be sodium sulfate of polyethenoxy ether of fatty alcohol, diethylene glycol, haloflex according to 2:3:6 mass ratio
Composed mixture.
6. the preparation method of the textile material according to claim 1 added with graphene, which is characterized in that the step
(6) concentration of finishing agent in water is 1wt% in.
7. any one of -6 preparation methods textile material obtained added with graphene is in medical dress ornament according to claim 1
Application in industry.
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