CN107245769A - A kind of garment material of graphene-containing and preparation method thereof - Google Patents
A kind of garment material of graphene-containing and preparation method thereof Download PDFInfo
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- CN107245769A CN107245769A CN201710490155.1A CN201710490155A CN107245769A CN 107245769 A CN107245769 A CN 107245769A CN 201710490155 A CN201710490155 A CN 201710490155A CN 107245769 A CN107245769 A CN 107245769A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent 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
- D01F6/92—Monocomponent 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
-
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
- 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
Abstract
The invention discloses a kind of garment material of graphene-containing and preparation method thereof, the garment material of the graphene-containing includes following raw material：PCL, PLA, graphene, imidazoline, the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type compatilizer, 1098 type antioxidant, propyl trimethoxy silicane, citrate, polybutadiene rubber, aluminium polychloride, ester based quaternary ammonium salt class softening agent, styrene, modified alta-mud heat stabilizer；Boric acid, lithium carbonate, fire retardant, the garment material of the graphene-containing are made by crushing, filling the steps such as energy, activation, wire drawing, cutting volume.The garment material of the present invention has two kinds of performances of high-hydroscopicity and quick hydrofuge, and hydroscopicity and scattered wet rate are significantly higher than the hydroscopicity of prior art and dissipate wet rate；The garment material of the present invention meets the requirement of Green Textiles, can be applicable.
Description
【Technical field】
The invention belongs to garment material preparing technical field, and in particular to a kind of garment material of graphene-containing and its preparation
Method.
【Background technology】
With the continuous progress of society, people require more and more high to the comfortableness of dress, and the comfortableness of clothes can be divided into
Comfortableness and psychological comfortableness physiologically.Comfortableness physiologically include hygroscopicity, gas permeability, warmth retention property, flexibility,
Retractility, weight and chemically etc., they are determined by the material property of making clothes；Psychological comfortableness bag
Adaptability of color, gloss, style, wrinkle resistance, stiffness, pilling resistance and environment etc. is included, wherein the property of many outward appearances
Can, it is also to be determined by the performance of dress materials.In recent years, people to the comfortableness of garment material, health, security and
Feature of environmental protection etc. requires more and more higher, and with the increase of people's activity time out of doors, easy dress is interpenetrated and melted with gym suit
The trend being integrated also increasingly is favored by consumers in general, the fabric of this kind of clothes, has both required good comfortableness, again
Ask in activity heartily, once there is situation soaked with sweat, clothes will not paste skin and produce cold wet feeling.
Hygroscopicity refers to the ability that object absorbs or released vaporous water in atmosphere, specifically just refers to dress materials energy
The sweat and steam of human skin's discharge are absorbed in time, and the another side of fabric can be passed to by fiber, are discharged into air
In ability.This performance is better, and hygroscopicity is better, and human body skin is drier, and people does not have feeling of oppression and heat, especially sultry
When summer and strenuous exercise.Gas permeability refers to the ability of gas permeation fabric.There is certain gas permeability as garment material, because
Also breathed all the time for human body skin, and the extraneous exchange for carrying out gas, there is the coming off of scurf, sweat fat daily
Discharge, for hygienic angle, garment material material will have certain gas permeability, be conducive to the exchange of gas inside and outside fabric,
Be conducive to the metabolism of human body skin.The dress materials gas permeability of particularly summer is the bigger the better, and is conducive to human heat's
Distribute, people then feels cool and comfortable.
Strength, wearability, resilience and the dimensional stability of polyester fiber can preferably meet the need of various final uses
Will, but polyester fiber is a kind of typical hydrophobic fibre, hydroscopicity only has 0.4%, is used as skintight suit material, its dress
Comfortableness is very poor, and especially when perspiring, it perspires difficulty, gives people sultry uncomfortable sensation.During polyester fiber is synthetic fibers
Yield is maximum, purposes most wide fiber species, by modification, has positive meaning using polyester fiber exploitation garment material.
Significantly affect human body comfort is the comprehensive radiating of garment material, scattered wet performance, and the key of garment material is water
Dividing can will quickly absorb, discharge, in general, and either natural fiber or synthetic fibers are all difficult to have water imbibition concurrently and fast
Both performances of fast hydrofuge, for unmodified polyester fiber hydroscopicity and dissipate the problem of wet rate is low, by how to be modified, make
Modified polyester fiber possesses high hydroscopicity and both performances of scattered wet rate, becomes new research direction.
【The content of the invention】
The present invention provides a kind of garment material of graphene-containing and preparation method thereof, to solve existing polyester fiber hygroscopicity
It is very poor, cause easily to gather electrostatic, easily inhale dust, the problems such as stain of going to degrease is difficult.
To solve above technical problem, the present invention uses following technical scheme：
A kind of garment material of graphene-containing, in units of parts by weight, including following raw material：200-320 parts of PCL, PLA
90-120 parts, 1-2 parts of graphene, 2-4 parts of the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, 1-2 parts of vanadic anhydride, ACR adjust
Save 5-8 parts of agent, 3-6 parts of aerogel generating agent, 12-16 parts of KH550 type silane couplers, 8-12 parts of acrylic type compatilizer,
It is 1098 3-5 parts of type antioxidant, 4-7 parts of propyl trimethoxy silicane, 6-12 parts of citrate, 9-15 parts of polybutadiene rubber, poly-
Close 5-9 parts of aluminium chloride, 15-22 parts of ester based quaternary ammonium salt class softening agent, 2-4 parts of styrene, 2-4 parts of modified alta-mud heat stabilizer；
3-6 parts of boric acid, 2-5 parts of lithium carbonate, 3-6 parts of fire retardant；
The fire retardant is in units of parts by weight, including following raw material：18-26 parts of 2-Butoxyethyl acetate, phosphoric acid hydrogen
Two 12-15 parts of ammoniums, 5-10 parts of aluminium hydroxide, 6-9 parts of antimony oxide, 4-6 parts of silane, 3-5 parts of kaolin, fatty alcohol polyoxy second
1.2-2 parts of alkene ether.
Preferably, the garment material of described graphene-containing, in units of parts by weight, in addition to following raw material：Live on surface
Property 0.3-0.5 parts of agent, the surfactant be imidazoline.
The present invention also provides a kind of preparation method of the garment material of graphene-containing, comprises the following steps：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -90-- in temperature
Primary comminution thing is crushed into 1.5-2.5h at 110 DEG C, the particulate of 400-600 mesh is obtained after sieving；
S3：Graphene is crushed, 200-400 mesh sieve is crossed, powder is made, gained powder is 5500- in magnetic field intensity
6500GS, ultrasonic power is 260-550W, and temperature is 42-53 DEG C, under rotating speed is 200-300r/min, stirs 18-37min,
Graphene energy powder is made；
S4：Imidazoline is added into graphene energy powder made from step S3, is 55-74 DEG C in temperature, rotating speed is 80-
0.9-1.6h is activated under 140r/min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (third of azo two made from step S2 are added into graphene energy powder made from step S4
Olefin(e) acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type phase
Hold agent, the mixing of 1098 type antioxidant and be warming up to 132-145 DEG C, stir 2-4h in the case where rotating speed is 200-300r/min, material is made
A；
S6：Propyl trimethoxy silicane is added into material A made from step S5, it is citrate, polybutadiene rubber, poly-
152-168 DEG C is warming up to after closing aluminium chloride, the mixing of ester based quaternary ammonium salt class softening agent, 1- is stirred in the case where rotating speed is 400-500r/min
1.5h, is made material B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, resistance
120-125 DEG C is cooled to after combustion agent mixing, 0.6-0.9h is stirred in the case where rotating speed is 200-300r/min, material C is made；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 220-260 DEG C, by high pressure screw rod
Melt is delivered to filter and filtered by extruder；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then through spinning group
Part sprays melt, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 36-44
28-42min is toasted under DEG C environment, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant is using 3 sections of warm areas
Temperature control method carry out, the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 9-32min；Second temperature
The temperature in degree area is gradually decremented to 67 DEG C from 82 DEG C, and time control is in 38-52min；The temperature of 3rd humidity province from 67 DEG C gradually
78 DEG C are incremented to, time control is in 18-48min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
Preferably, the preparation method of fire retardant described in step S7, comprises the following steps：
S71：Diammonium hydrogen phosphate, 80-100 parts of water are added in microwave reactor, are 200-300r/min in speed of agitator
Lower stirring 10-14min, is made mixture a；
S72：Into mixture a made from step S71 add 2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide,
Silane, kaolin, AEO, are 300-500r/min in speed of agitator, microwave power is 250-300W, temperature
To stir 1-1.5h at 88-92 DEG C, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 3000- in rotating speed
Fire retardant is made to water content≤2.5% in centrifugal drying under 5000r/min.
The invention has the advantages that：
(1) garment material of the invention has two kinds of performances of high-hydroscopicity and quick hydrofuge, and hydroscopicity and scattered wet rate show
Write the hydroscopicity and scattered wet rate higher than prior art；
(2) played from embodiment 3 and comparative example 1-3 data, graphene and imidazoline in garment material is prepared
Synergy, improves hydroscopicity and dissipates wet rate；
(3) from embodiment 3 and comparative example 4-6 data, step S3 and step S4 of the present invention graphene fill and can located
Reason and activation process also play synergy in garment material is prepared, and improve hydroscopicity and dissipate wet rate；
(4) garment material of the invention meets the requirement of Green Textiles, can be applicable.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following examples, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In embodiment, the garment material of the graphene-containing, it is characterised in that in units of parts by weight, including it is following
Raw material：200-320 parts of PCL, 90-120 parts of PLA, 1-2 parts of graphene, 0.3-0.5 parts of imidazoline, the isobutyric acid (propylene of azo two
Sour ethylene glycol) 2-4 parts of ester, 1-2 parts of vanadic anhydride, 5-8 parts of ACR conditioning agents, 3-6 parts of aerogel generating agent, KH550 type silane
12-16 parts of coupling agent, 8-12 parts of acrylic type compatilizer, 3-5 parts of 1098 type antioxidant, 4-7 parts of propyl trimethoxy silicane, lemon
6-12 parts of lemon acid esters, 9-15 parts of polybutadiene rubber, 5-9 parts of aluminium polychloride, 15-22 parts of ester based quaternary ammonium salt class softening agent, benzene
2-4 parts of ethene, 2-4 parts of modified alta-mud heat stabilizer；3-6 parts of boric acid, 2-5 parts of lithium carbonate, 3-6 parts of fire retardant.
The fire retardant is in units of parts by weight, including following raw material：18-26 parts of 2-Butoxyethyl acetate, phosphoric acid hydrogen
Two 12-15 parts of ammoniums, 5-10 parts of aluminium hydroxide, 6-9 parts of antimony oxide, 4-6 parts of silane, 3-5 parts of kaolin, fatty alcohol polyoxy second
1.2-2 parts of alkene ether.
The preparation method of the garment material of the graphene-containing, comprises the following steps：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -90-- in temperature
Primary comminution thing is crushed into 1.5-2.5h at 110 DEG C, the particulate of 400-600 mesh is obtained after sieving；
S3：Graphene is crushed, 200-400 mesh sieve is crossed, powder is made, gained powder is 5500- in magnetic field intensity
6500GS, ultrasonic power is 260-550W, and temperature is 42-53 DEG C, under rotating speed is 200-300r/min, stirs 18-37min,
Graphene energy powder is made；
S4：Imidazoline is added into graphene energy powder made from step S3, is 55-74 DEG C in temperature, rotating speed is 80-
0.9-1.6h is activated under 140r/min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (third of azo two made from step S2 are added into graphene energy powder made from step S4
Olefin(e) acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type phase
Hold agent, the mixing of 1098 type antioxidant and be warming up to 132-145 DEG C, stir 2-4h in the case where rotating speed is 200-300r/min, material is made
A；
S6：Propyl trimethoxy silicane is added into material A made from step S5, it is citrate, polybutadiene rubber, poly-
152-168 DEG C is warming up to after closing aluminium chloride, the mixing of ester based quaternary ammonium salt class softening agent, 1- is stirred in the case where rotating speed is 400-500r/min
1.5h, is made material B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, resistance
120-125 DEG C is cooled to after combustion agent mixing, 0.6-0.9h is stirred in the case where rotating speed is 200-300r/min, material C is made；
The preparation method of fire retardant, comprises the following steps described in step S7：
S71：Diammonium hydrogen phosphate, 80-100 parts of water are added in microwave reactor, are 200-300r/min in speed of agitator
Lower stirring 10-14min, is made mixture a；
S72：Into mixture a made from step S71 add 2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide,
Silane, kaolin, AEO, are 300-500r/min in speed of agitator, microwave power is 250-300W, temperature
To stir 1-1.5h at 88-92 DEG C, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 3000- in rotating speed
Fire retardant is made to water content≤2.5% in centrifugal drying under 5000r/min；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 220-260 DEG C, by high pressure screw rod
Melt is delivered to filter and filtered by extruder；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then through spinning group
Part sprays melt, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 36-44
28-42min is toasted under DEG C environment, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant is using 3 sections of warm areas
Temperature control method carry out, the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 9-32min；Second temperature
The temperature in degree area is gradually decremented to 67 DEG C from 82 DEG C, and time control is in 38-52min；The temperature of 3rd humidity province from 67 DEG C gradually
78 DEG C are incremented to, time control is in 18-48min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of garment material of graphene-containing, it is characterised in that in units of parts by weight, including following raw material：PCL 280
Part, 100 parts of PLA, 1.6 parts of graphene, 0.4 part of imidazoline, 3 parts of the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, five oxidations two
1.6 parts of vanadium, 6 parts of ACR conditioning agents, 5 parts of aerogel generating agent, 14 parts of KH550 types silane coupler, acrylic type compatilizer 10
Part, 4 parts of 1098 type antioxidant, 6 parts of propyl trimethoxy silicane, 10 parts of citrate, 12 parts of polybutadiene rubber, polyaluminium
8 parts of aluminium, 18 parts of ester based quaternary ammonium salt class softening agent, 3 parts of styrene, 3 parts of modified alta-mud heat stabilizer；4 parts of boric acid, lithium carbonate 4
Part, 5 parts of fire retardant.
The fire retardant is in units of parts by weight, including following raw material：22 parts of 2-Butoxyethyl acetate, diammonium hydrogen phosphate
13 parts, 8 parts of aluminium hydroxide, 8 parts of antimony oxide, 5 parts of silane, 4 parts of kaolin, 1.6 parts of AEO.
The preparation method of the garment material of the graphene-containing, comprises the following steps：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -100 in temperature
Primary comminution thing is crushed into 2h at DEG C, the particulate of 500 mesh is obtained after sieving；
S3：Graphene is crushed, 300 mesh sieve are crossed, powder is made, gained powder is 6000GS, ultrasound in magnetic field intensity
Wave power is 420W, and temperature is 48 DEG C, and graphene energy powder is made under 250r/min, to stir 26min in rotating speed；
S4：Imidazoline is added into graphene energy powder made from step S3, is 65 DEG C in temperature, rotating speed is 120r/
1.3h is activated under min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (third of azo two made from step S2 are added into graphene energy powder made from step S4
Olefin(e) acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type phase
Hold agent, the mixing of 1098 type antioxidant and be warming up to 140 DEG C, stir 3h in the case where rotating speed is 250r/min, material A is made；
S6：Propyl trimethoxy silicane is added into material A made from step S5, it is citrate, polybutadiene rubber, poly-
160 DEG C are warming up to after closing aluminium chloride, the mixing of ester based quaternary ammonium salt class softening agent, 1.3h is stirred in the case where rotating speed is 450r/min, is made
Material B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, resistance
122 DEG C are cooled to after combustion agent mixing, 0.8h is stirred in the case where rotating speed is 250r/min, material C is made；
The preparation method of fire retardant, comprises the following steps described in step S7：
S71：Diammonium hydrogen phosphate, 90 parts of water are added in microwave reactor, stirred in the case where speed of agitator is 250r/min
12min, is made mixture a；
S72：Into mixture a made from step S71 add 2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide,
Silane, kaolin, AEO, are 400r/min in speed of agitator, microwave power is 280W, and temperature is at 90 DEG C
1.3h is stirred, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 4000r/min in rotating speed
Lower centrifugal drying to water content is 2.5%, and fire retardant is made；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 250 DEG C, by high pressure screw extruding
Melt is delivered to filter and filtered by machine；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then through spinning group
Part sprays melt, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 40 DEG C of rings
35min is toasted under border, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant is using 3 sections of warm areas
Temperature control method carry out, the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 20min；Second temperature
The temperature in area is gradually decremented to 67 DEG C from 82 DEG C, and time control is in 45min；The temperature of 3rd humidity province is gradually incremented to from 67 DEG C
78 DEG C, time control is in 32min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
Embodiment 2
A kind of garment material of graphene-containing, it is characterised in that in units of parts by weight, including following raw material：PCL 200
Part, 95 parts of PLA, 1.1 parts of graphene, 0.3 part of imidazoline, 2 parts of the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, five oxidations two
1 part of vanadium, 5 parts of ACR conditioning agents, 3 parts of aerogel generating agent, 12 parts of KH550 types silane coupler, 8 parts of acrylic type compatilizer,
1098 3 parts of type antioxidant, 4 parts of propyl trimethoxy silicane, 6 parts of citrate, 9 parts of polybutadiene rubber, aluminium polychloride 5
Part, 15 parts of ester based quaternary ammonium salt class softening agent, 2 parts of styrene, 2 parts of modified alta-mud heat stabilizer；3 parts of boric acid, 3 parts of lithium carbonate,
3 parts of fire retardant.
The fire retardant is in units of parts by weight, including following raw material：20 parts of 2-Butoxyethyl acetate, diammonium hydrogen phosphate
12 parts, 6 parts of aluminium hydroxide, 6 parts of antimony oxide, 4 parts of silane, 3 parts of kaolin, 1.5 parts of AEO.
The preparation method of the garment material of the graphene-containing, comprises the following steps：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -90 DEG C in temperature
It is lower that primary comminution thing is crushed into 2.5h, the particulate of 400 mesh is obtained after sieving；
S3：Graphene is crushed, 200 mesh sieve are crossed, powder is made, gained powder is 5500GS, ultrasound in magnetic field intensity
Wave power is 260W, and temperature is 42 DEG C, and graphene energy powder is made under 200r/min, to stir 37min in rotating speed；
S4：Imidazoline is added into graphene energy powder made from step S3, is 55 DEG C in temperature, rotating speed is 80r/
1.6h is activated under min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (third of azo two made from step S2 are added into graphene energy powder made from step S4
Olefin(e) acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type phase
Hold agent, the mixing of 1098 type antioxidant and be warming up to 132 DEG C, stir 4h in the case where rotating speed is 200r/min, material A is made；
S6：Propyl trimethoxy silicane is added into material A made from step S5, it is citrate, polybutadiene rubber, poly-
152 DEG C are warming up to after closing aluminium chloride, the mixing of ester based quaternary ammonium salt class softening agent, 1.5h is stirred in the case where rotating speed is 400r/min, is made
Material B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, resistance
120 DEG C are cooled to after combustion agent mixing, 0.9h is stirred in the case where rotating speed is 200r/min, material C is made；
The preparation method of fire retardant, comprises the following steps described in step S7：
S71：Diammonium hydrogen phosphate, 80 parts of water are added in microwave reactor, stirred in the case where speed of agitator is 200r/min
14min, is made mixture a；
S72：Into mixture a made from step S71 add 2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide,
Silane, kaolin, AEO, are 300r/min in speed of agitator, microwave power is 250W, and temperature is at 88 DEG C
1.5h is stirred, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 3000r/min in rotating speed
Lower centrifugal drying to water content is 2%, and fire retardant is made；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 220 DEG C, by high pressure screw extruding
Melt is delivered to filter and filtered by machine；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then through spinning group
Part sprays melt, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 36 DEG C of rings
42min is toasted under border, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant is using 3 sections of warm areas
Temperature control method carry out, the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 32min；Second temperature
The temperature in area is gradually decremented to 67 DEG C from 82 DEG C, and time control is in 38min；The temperature of 3rd humidity province is gradually incremented to from 67 DEG C
78 DEG C, time control is in 18min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
Embodiment 3
A kind of garment material of graphene-containing, it is characterised in that in units of parts by weight, including following raw material：PCL 300
Part, 120 parts of PLA, 1.9 parts of graphene, 0.5 part of imidazoline, 4 parts of the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, five oxidations two
2 parts of vanadium, 8 parts of ACR conditioning agents, 6 parts of aerogel generating agent, 16 parts of KH550 types silane coupler, 12 parts of acrylic type compatilizer,
1098 5 parts of type antioxidant, 7 parts of propyl trimethoxy silicane, 12 parts of citrate, 15 parts of polybutadiene rubber, aluminium polychloride 9
Part, 22 parts of ester based quaternary ammonium salt class softening agent, 4 parts of styrene, 4 parts of modified alta-mud heat stabilizer；6 parts of boric acid, 5 parts of lithium carbonate,
6 parts of fire retardant.
The fire retardant is in units of parts by weight, including following raw material：26 parts of 2-Butoxyethyl acetate, diammonium hydrogen phosphate
15 parts, 10 parts of aluminium hydroxide, 9 parts of antimony oxide, 6 parts of silane, 5 parts of kaolin, 2 parts of AEO.
The preparation method of the garment material of the graphene-containing, comprises the following steps：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -110 in temperature
Primary comminution thing is crushed into 1.5h at DEG C, the particulate of 600 mesh is obtained after sieving；
S3：Graphene is crushed, 400 mesh sieve are crossed, powder is made, gained powder is 6500GS, ultrasound in magnetic field intensity
Wave power is 550W, and temperature is 53 DEG C, and graphene energy powder is made under 300r/min, to stir 18min in rotating speed；
S4：Imidazoline is added into graphene energy powder made from step S3, is 74 DEG C in temperature, rotating speed is 140r/
0.9h is activated under min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (third of azo two made from step S2 are added into graphene energy powder made from step S4
Olefin(e) acid ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type phase
Hold agent, the mixing of 1098 type antioxidant and be warming up to 145 DEG C, stir 2h in the case where rotating speed is 300r/min, material A is made；
S6：Propyl trimethoxy silicane is added into material A made from step S5, it is citrate, polybutadiene rubber, poly-
168 DEG C are warming up to after closing aluminium chloride, the mixing of ester based quaternary ammonium salt class softening agent, 1h is stirred in the case where rotating speed is 500r/min, thing is made
Expect B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, resistance
125 DEG C are cooled to after combustion agent mixing, 0.6h is stirred in the case where rotating speed is 300r/min, material C is made；
The preparation method of fire retardant, comprises the following steps described in step S7：
S71：Diammonium hydrogen phosphate, 100 parts of water are added in microwave reactor, stirred in the case where speed of agitator is 300r/min
10min, is made mixture a；
S72：Into mixture a made from step S71 add 2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide,
Silane, kaolin, AEO, are 500r/min in speed of agitator, microwave power is 300W, and temperature is at 92 DEG C
1h is stirred, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 5000r/min in rotating speed
Lower centrifugal drying to water content is 1.8%, and fire retardant is made；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 260 DEG C, by high pressure screw extruding
Melt is delivered to filter and filtered by machine；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then through spinning group
Part sprays melt, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 44 DEG C of rings
28min is toasted under border, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant is using 3 sections of warm areas
Temperature control method carry out, the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 9min；Second temperature area
Temperature be gradually decremented to 67 DEG C from 82 DEG C, time control is in 52min；The temperature of 3rd humidity province is gradually incremented to 78 from 67 DEG C
DEG C, time control is in 48min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
Comparative example 1
Preparation technology is essentially identical with implementing 3, and it is not both that preparing raw material lacks graphene and imidazoline to have only.
Comparative example 2
Preparation technology is essentially identical with implementing 3, and it is not both that preparing raw material lacks graphene to have only.
Comparative example 3
Preparation technology is essentially identical with implementing 3, and it is not both that preparing raw material lacks imidazoline to have only.
Comparative example 4
Preparation technology is essentially identical with implementing 3, and it is not both to fill to locate without step S3 and step S4 graphene to have only
Reason and activation process.
Comparative example 5
Preparation technology is essentially identical with implementing 3, and it is not both to fill to handle without step S3 graphene to have only.
Comparative example 6
Preparation technology and implement 3 essentially identical, it is not both graphene activation process without step S4 to have only.
Comparative example 7
Using a kind of Chinese patent application document " manufacture method of the garment material " (patent No.：200910101498.X) real
The method for applying a 1-3 prepares garment material.
In the case where condition is essentially identical, detects the hydroscopicity of garment material made from embodiment 1-3 and comparative example 1-7 and dissipate wet
Rate is detected, as a result as shown in the table.
By upper table it is recognised that the hydroscopicity of garment material produced by the present invention and scattered wet rate are significantly higher than prior art
Hydroscopicity and scattered wet rate；
From embodiment 3 and comparative example 1-3 data, graphene and imidazoline serve association in garment material is prepared
Same-action, improves hydroscopicity and dissipates wet rate；
From embodiment 3 and comparative example 4-6 data, step S3 and step S4 graphene fill can handle and activation at
Reason serves synergy in garment material is prepared, and improves hydroscopicity and dissipates wet rate.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (4)
1. a kind of garment material of graphene-containing, it is characterised in that in units of parts by weight, including following raw material：PCL 200-
320 parts, 90-120 parts of PLA, 1-2 parts of graphene, 2-4 parts of the isobutyric acid of azo two (acrylic acid ethylene glycol) ester, vanadic anhydride 1-
2 parts, 5-8 parts of ACR conditioning agents, 3-6 parts of aerogel generating agent, 12-16 parts of KH550 type silane couplers, acrylic type compatilizer
8-12 parts, 3-5 parts of 1098 type antioxidant, 4-7 parts of propyl trimethoxy silicane, 6-12 parts of citrate, polybutadiene rubber 9-
15 parts, 5-9 parts of aluminium polychloride, 15-22 parts of ester based quaternary ammonium salt class softening agent, 2-4 parts of styrene, modified alta-mud heat stabilizer
2-4 parts；3-6 parts of boric acid, 2-5 parts of lithium carbonate, 3-6 parts of fire retardant；
The fire retardant is in units of parts by weight, including following raw material：18-26 parts of 2-Butoxyethyl acetate, diammonium hydrogen phosphate
12-15 parts, 5-10 parts of aluminium hydroxide, 6-9 parts of antimony oxide, 4-6 parts of silane, 3-5 parts of kaolin, AEO
1.2-2 part.
2. the garment material of graphene-containing according to claim 1, it is characterised in that in units of parts by weight, in addition to
Following raw material：0.3-0.5 parts of surfactant, the surfactant is imidazoline.
3. a kind of preparation method of the garment material of graphene-containing according to claim 2, it is characterised in that including following
Step：
S1：PCL, PLA are subjected to mixing preliminary crushing using disintegrating machine, primary comminution thing is made；
S2：Primary comminution thing made from step S1 is placed in the Lowtemperaturepulverizer of nitrogen or dry ice, is -90--110 in temperature
Primary comminution thing is crushed into 1.5-2.5h at DEG C, the particulate of 400-600 mesh is obtained after sieving；
S3：Graphene is crushed, 200-400 mesh sieve is crossed, powder is made, gained powder is 5500-6500GS in magnetic field intensity,
Ultrasonic power is 260-550W, and temperature is 42-53 DEG C, and graphite is made under 200-300r/min, to stir 18-37min in rotating speed
Alkene energy powder；
S4：Imidazoline is added into graphene energy powder made from step S3, is 55-74 DEG C in temperature, rotating speed is 80-
0.9-1.6h is activated under 140r/min, activated graphene energy powder is made；
S5：Particulate, the isobutyric acid (acrylic acid of azo two made from step S2 are added into graphene energy powder made from step S4
Ethylene glycol) ester, vanadic anhydride, ACR conditioning agents, aerogel generating agent, KH550 types silane coupler, acrylic type compatilizer,
The mixing of 1098 type antioxidant is warming up to 132-145 DEG C, stirs 2-4h in the case where rotating speed is 200-300r/min, material A is made；
S6：Propyl trimethoxy silicane, citrate, polybutadiene rubber, polymerization chlorine are added into material A made from step S5
152-168 DEG C is warming up to after changing aluminium, the mixing of ester based quaternary ammonium salt class softening agent, 1- is stirred in the case where rotating speed is 400-500r/min
1.5h, is made material B；
S7：Styrene, modified alta-mud heat stabilizer are added into material B made from step S6；Boric acid, lithium carbonate, fire retardant
120-125 DEG C is cooled to after mixing, 0.6-0.9h is stirred in the case where rotating speed is 200-300r/min, material C is made；
S8：Material C made from step S7 is changed into liquid from solid-state in the case where temperature is 220-260 DEG C, by high pressure screw extruding
Melt is delivered to filter and filtered by machine；
S9：Melt after filtering is further well mixed, makes its viscosity consistent, strengthens spinnability, then will through filament spinning component
Melt is sprayed, then the tow that spinning sprays is wound into cylinder, then drawing fiber silk；
S10：Filament made from step S9 is prepared into cloth using conventional method, by the cloth prepared in 36-44 DEG C of ring
28-42min is toasted under border, then takes out that to naturally cool to normal temperature stand-by；
S11：Normal temperature cloth feeding drying plant will be cooled in step S10, the temperature of drying plant uses the control of 3 sections of warm areas
Warm mode is carried out, and the temperature of the first humidity province is gradually incremented to 82 DEG C from 68 DEG C, and time control is in 9-32min；Second temperature area
Temperature be gradually decremented to 67 DEG C from 82 DEG C, time control is in 38-52min；The temperature of 3rd humidity province is gradually incremented by from 67 DEG C
To 78 DEG C, time control is in 18-48min；
S12：Obtained cloth in step S11 is subjected to shaping cutting, garment material is made.
4. the preparation method of the garment material of graphene-containing according to claim 3, it is characterised in that described in step S7
The preparation method of fire retardant, comprises the following steps：
S71：Diammonium hydrogen phosphate, 80-100 parts of water are added in microwave reactor, stirred in the case where speed of agitator is 200-300r/min
10-14min is mixed, mixture a is made；
S72：2-Butoxyethyl acetate, aluminium hydroxide, antimony oxide, silicon are added into mixture a made from step S71
Alkane, kaolin, AEO, are 300-500r/min in speed of agitator, microwave power is 250-300W, and temperature is
1-1.5h is stirred at 88-92 DEG C, mixture b is made；
S73：Mixture b made from step S72 is cooled to after room temperature, sediment is filtered, is 3000-5000r/ in rotating speed
Fire retardant is made to water content≤2.5% in centrifugal drying under min.
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| CN109881497A (en) * | 2019-02-25 | 2019-06-14 | 朱建余 | A kind of waterproof fabrics and preparation method thereof |
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