CN105543993A - Graphene modified color paste, preparation method and application - Google Patents
Graphene modified color paste, preparation method and application Download PDFInfo
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- CN105543993A CN105543993A CN201610021013.6A CN201610021013A CN105543993A CN 105543993 A CN105543993 A CN 105543993A CN 201610021013 A CN201610021013 A CN 201610021013A CN 105543993 A CN105543993 A CN 105543993A
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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
- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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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
- 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
- D01F1/04—Pigments
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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
- 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
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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
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to graphene modified color paste. The graphene modified color paste is prepared from, by weight, 0.1-5% of graphene, 15-55% of carbon black, 2-25% of functional aids, 2-20% of a dispersing agent and the balance a solvent. By adding the specific amount of graphene into the color paste containing the specific amount of carbon black, the carbon block is attached to the surface of the graphene, dispersion of graphene can be facilitated because of the binding force between the carbon black and the graphene, and the defect that the graphene is not uniform in dispersion after being added into spinning liquid. Besides, the binding force between the specific amount of graphene and the specific amount of carbon black disappears in the spinning process, the functions of graphene in obtained textiles are give play to, and the textiles have the characteristics, such as excellent far infrared performance, bacteria resistance and the bacteriostasis and ultraviolet resistance, of graphene.
Description
Technical field
The invention belongs to technical field of dye, relate to a kind of mill base, be specifically related to a kind of Graphene modification mill base, preparation method and its usage.
Background technology
Graphene is SP between carbon atom
2hydridization Cheng Jian, be arranged in the monoatomic layer flat crystal of bi-dimensional cellular shape lattice, it has bigger serface, excellent electricity, calorifics and mechanical property.At present, Graphene attracts the characteristic of researcher to be the mechanical property of its excellence most.Graphene is the material that mankind's known strength is the highest, also harder than diamond, taller upper 100 times of the iron and steel that strength ratio is best in the world.Using Graphene and matrix polymer compound to prepare composite or fiber, obviously can improve the performance of material, as improved physical-mechanical properties, improving electricity and heat resistance etc.
Technology of preparing about Graphene hybrid polymer thing composite has been reported, and the method preparing Graphene/polymer composites at present mainly contains: solution blended process, mechanical blending method and situ aggregation method.CN101462889A, is prepared from the graphene coated coating in carbon fibre material surface by the method for coating for raw material with Graphene and carbon fibre material.CN101474897A, to be layering film forming by method for manufacturing thin film such as spin coating, spraying, dipping-lifts for raw material with grapheme material and organic material.Graphene/the polyimide composite film (D.Chen, H.ZhuandT.X.Liu, AcsApplMaterInter, 2. (2010) .) of the excellent in mechanical performance that utilized solution blended process to prepare such as Chen Dan.Wang etc. have prepared low-k by in-situ polymerization, the graphene oxide of excellent in mechanical performance/polyimide composite film (.J.Y.Wang, S.Y.Yang, Y.L.Huang, H.W.Tien, W.K.ChinandC.C.M.Ma, JMaterChem, 21. (2011)).Luong, N.D. etc., by in-situ polymerization, have prepared Graphene/polyimide composite film, improve the mechanical property of Kapton, improve its electric conductivity, the mechanical property after improvement reaches 2.3GPa (N.D.Luong, U.Hippi, J.T.Korhonen, A.J.Soininen, J.Ruokolainen, L.S.Johansson, J.D.Nam, L.H.SinhandJ.Seppala, Polymer, 52. (2011) .).
Solution dyeing refers in polymer processing or after process, adds the production method that colouring agent obtains colored fibre before spinning.Compared with common staining method, solution dyeing primary colours fastness is high, and post processing is also simpler, is subject to the welcome in market.Original liquid coloring fiber in spinning solution, adds graining paste carry out the obtained fiber of spinning.The spinning process of viscose glue long and short fiber manufacturer is generally utilized by a certain percentage by mill base to spin front static mixing injector and join in spinning solution, sprayed with certain speed by the duct of spinning head, coloured stoste thread solidifies with coagulating bath in coagulating bath, decompose, regenerative response and generate as-spun fibre, by drawing-off and post processing, complete the spinning of colored fibre.And granules of pigments size directly affects the tone of color, the processing granularity of pigment should below 1.0 microns.Pigment particle size is thinner, and particle size distribution range is narrower, and brightness and the purity of color are higher; And the granularity of pigment is larger, coloured light scattering is more obvious, color homogeneity and painted fastness also poorer.By the addition of pigment 1.5 ~ 3.0%, when pigment particle size is greater than 1/50 of fibre diameter, just there will be coloured light scattering.In addition, if the dispersing uniformity of the pigment of graining paste in viscose glue is poor, pigment can by the stoste wrapping agglomeration (moisture in adsorption pigment slurry, reduce intersolubility), the granularity of pigment under practical stability state is caused to increase and skewness, also more important than pigment itself on the impact of fiber colour uniformity.Therefore, pigment slurry should impose strong shear plasticizing in time.The research of prior art proves, must stabilizing technical processes as much as possible, ensures that technological parameter fluctuates in more among a small circle, could improve stock-dye uniformity.
Existing Graphene is used for spinning and prepares textiles mainly by being added spinning solution, and then spinning obtains the textiles of Graphene modification.But in the method, Graphene disperses uneven in spinning solution, cause graphene dispersion in the textiles obtained uneven, effect of Graphene cannot be played well.In addition, in process prepared by colored textiles, pigment is coated graphite alkene very easily, causes Graphene in the textiles obtained coated by pigment completely, and cannot play its effect.
Summary of the invention
For Problems existing in prior art, an object of the present invention is to provide a kind of Graphene modification mill base.By Graphene is added mill base, and then mill base is mixed with spinning solution carry out spinning, dispersed in textiles of Graphene can be realized, obtain the textiles of various aspects of performance excellence.
To achieve these goals, present invention employs following technical scheme:
A kind of Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
Surplus is solvent.
In the present invention, described mill base, except " Graphene, carbon black, function additive and dispersant ", can also comprise " other components ", and described " other components " can give described mill base different characteristics.Described " surplus is solvent " namely refers to, the component except above-mentioned " Graphene, carbon black, function additive and dispersant " and above-mentioned " other components " is solvent.
Graphene of the present invention refers to that the Graphene that conventional existing technique prepares, the Graphene that common process prepares are a kind of mixture of the carbon containing Graphene, may contain other allotropes of carbon, also may containing other mineral element.Such as, in the Graphene utilizing graphite ore to prepare for raw material, may containing some mineral element that in graphite ore, self exists.The living beings Graphene of indication is the Graphene utilizing biomass resource to prepare for raw material, also may can there is plant because self needing to absorb other allotropes of mineral element and the carbon obtained from soil.Therefore, in the present invention, the Graphene of indication is specially a kind of mixture containing Graphene.
The present invention is by adding in the mill base containing specific carbon black amount by the Graphene of specified quantitative, carbon black is made to be attached to the surface of Graphene, adhesion between the two can contribute to the dispersion of Graphene, avoids Graphene and adds in spinning solution the defect of disperseing inequality to.In addition, adhesion between the Graphene of specified quantitative and carbon black disappears in spinning process, effect of Graphene in the textiles obtained is played, makes textiles have the characteristic of Graphene, as the far infrared performance of excellence, antibacterial bacteriostatic performance and ultraviolet resistance.
The present invention is used by the collocation of Graphene and dispersant and function additive, further improve the dispersibility of Graphene, reach mill base mix with spinning solution after the object that improves of graphene dispersion, and make Graphene in the spinning product obtained distribute more even.
And the present invention is by introducing mill base by Graphene, then spinning after being mixed with weaving liquid by mill base, is easier to suitability for industrialized production, can adapts to the every physical and chemical changes in follow-up spinning process.
The content of described Graphene is 0.1 ~ 5%, as 0.3%, 0.5%, 0.8%, 1.1%, 1.4%, 1.7%, 2.0%, 2.3%, 2.6%, 2.9%, 3.2%, 3.5%, 3.8%, 4.1%, 4.4%, 4.7% or 4.9%, be preferably 0.1 ~ 3%, when can realize low cost, obtain the Graphene modification mill base of excellent performance.
Preferably, described Graphene raw materials is living beings.The present invention, by selecting living beings to be Graphene prepared by raw material, can make Graphene with bioactive ingredients.
The content of described carbon black is 15 ~ 55%, such as 17%, 18%, 19%, 20%, 21%, 22%, 23%, 25%, 27%, 29%, 31%, 33%, 35%, 37%, 39%, 41%, 43%, 45%, 47%, 49%, 51% or 53%, be preferably 20 ~ 35%.Can also be a little less again, outstanding is exactly a bit adding of Graphene, decreases the introducing of carbon black; Such as original carbon black loading is 40%, and add 1% Graphene, carbon black only just can reach original effect with 30%.
Preferably, the particle diameter of described carbon black is < 5 μm, is preferably less than 2 μm.
The content of described function additive is 2 ~ 25%, such as 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%, 21% or 23%, be preferably 5-15%, more preferably 10 ~ 15%.
Preferably, described function additive is propylene glycol monomethyl ether, EGME, dimethyl sulfoxide (DMSO) (it can promote the miscible of mill base and spinning solution in fabrication processes), dimethyl propylene glycol, glycerol, propylene glycol, ethylene glycol, polypropylene glycol, polyethylene glycol, dodecyl benzyl dimethyl ammonium chloride, cellulose ether, isothiazolinone, bohr ripple is many, the combination of any one or at least two kinds in click conifer antimildew disinfectant or defoamer, preferred propylene glycol monomethyl ether, EGME, dimethyl sulfoxide (DMSO), dimethyl propylene glycol, glycerol, propylene glycol, ethylene glycol, the combination of any one or at least two kinds in polypropylene glycol or polyethylene glycol, it can play the effect alleviating mill base sedimentation and flocculation.
Preferably, described defoamer is the combination of any one or at least two kinds in mineral oil antifoam agent, phosphate defoamer, fat hydrocarbon defoamer or silicone oil defoamer.
The content of described dispersant is 2 ~ 20%, such as 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18% or 19%, preferably 5 ~ 15%.
Preferably, described dispersant is the mixture of any one or at least two kinds in ammonium polyacrylate salt, polyacrylic acid sodium salt, di-2-ethylhexylphosphine oxide first sodium naphthalene sulfonate, benzyl naphthalenesulfonate formaldehyde condensation compound, naphthalenesulfonic acid-formaldehyde condensate, sulfocarbolate formaldehyde condensation products, phenolic aldehyde polyoxyethylene ether, polyoxyethylene ether, derivative of fatty acid, polyacrylate, modified polyacrylate, alkyl sulfate or alkyl sulfonate compound.
Preferably, described solvent is that DMF is or/and deionized water.
Preferably, described mill base also comprises pH adjusting agent.
Preferably, described pH adjusting agent is NaOH, KOH, NH
3h
2o, CH
3cOOH, Co (NH
2)
2, HCON (CH
3)
2, 1-METHYLPYRROLIDONE, any one or at least two kinds in NOP or triethanolamine mixture.
Preferably, add pH adjusting agent to regulate pH to 7 ~ 11 of mill base, the pH preferably regulating mill base is 7.The pH regulating mill base is 7, and spinning later stage sour environment can be avoided the impact of mill base.
Preferably, particle diameter≤0.2 μm of described mill base.
Two of object of the present invention is the preparation method providing a kind of Graphene modification mill base as above, comprises the following steps:
(1) by Graphene, carbon black, function additive, dispersant, solvent and optionally pH adjusting agent mixing, premixed carbon black is obtained;
(2) premixed carbon black is ground, obtain Graphene modification mill base.
In mill base preparation process; because grinding can destroy the molecular structure of Graphene, and the present invention is by selecting the addition of specific Graphene and carbon black, makes carbon black be attached to the surface of Graphene; carbon black plays the effect of protection Graphene, avoids the destruction of grinding to graphene-structured.
Preferably, step (1) obtains premixed carbon black and comprises the following steps:
A function additive adds in the mixed solution of solvent and dispersant by ();
B Graphene and carbon black add in the mixed solution that step (a) obtains by (), obtain the pre-dispersed slurry of carbon black;
C the pre-dispersed slurry of carbon black of gained in step (b) is not less than 30 minutes with the Rate Dispersion of 1500 ~ 3000r/min by (), and in dispersion process, slowly add pH value regulator control pH at 7-11, obtains premixed carbon black.
Preferably, the combination of micro-any one or at least two kinds penetrated in pulverizing or horizontal grinding of ball milling, basket grinding, homogeneous is ground to described in.
Preferably, premixed carbon black is ground, when its particle diameter reach≤0.2 μm time stop grinding.
Preferably, also comprise after stopping grinding, with the Rate Dispersion at least 15 minutes of 1500r/min, obtain the step of initial carbon black.
Preferably, also comprise initial carbon black quality testing, vacuum defoamation and the step that filters and packages.
Preferably, a kind of preparation method of Graphene modification mill base, comprises the following steps:
(1) solvent and dispersant are added in blender, with 500 ~ 700r/min Rate Dispersion 15 minutes, obtain the first mixed solution; Function additive is added in the first mixed solution and mix, obtain the second mixed solution; Graphene and carbon black are added the second mixed solution, obtains the pre-dispersed slurry of carbon black; Pre-dispersed for carbon black slurry is not less than 30 minutes with the Rate Dispersion of 1500 ~ 3000r/min, and in dispersion process, slowly adds pH value regulator control pH 7 ~ 11, obtain premixed carbon black;
(2) premixed carbon black is ground, when its particle diameter reach≤0.2 μm time stop grinding, with the Rate Dispersion 15 minutes of 1500r/min, obtain initial carbon black; Quality testing, vacuum defoamation and after filtering and packaging are carried out to initial carbon black, obtains Graphene modification mill base.
Three of object of the present invention is the purposes providing a kind of Graphene modification mill base as above, and it carries out spinning after mixing with spinning solution and prepares colored textiles.
It is painted that the mill base of gained of the present invention is specially adapted to viscose glue, acrylic fiber and paper pulp, is applicable to latex, sponge and water paint too painted.
Compared with the prior art, the present invention has following beneficial effect:
The present invention is by adding in the mill base containing specific carbon black amount by the Graphene of specified quantitative, carbon black is made to be attached to the surface of Graphene, adhesion between the two can contribute to the dispersion of Graphene, avoids Graphene and adds in spinning solution the defect of disperseing inequality to.Simultaneously, adhesion between the Graphene of specified quantitative and carbon black disappears in spinning process, effect of Graphene in the textiles obtained is played, makes textiles have the characteristic of Graphene, as the far infrared performance of excellence, antibacterial bacteriostatic performance and ultraviolet resistance.
The present invention is by Graphene and use with the collocation of dispersant and function additive, further improve the dispersibility of Graphene, reach mill base mix with spinning solution after the object that improves of graphene dispersion, and make Graphene in the spinning product obtained distribute more even.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below by detailed description of the invention.
In following embodiment and comparative example, described Graphene raw materials is living beings, and the living beings Graphene prepared has C/O at 93-98/2-7, and ash content is at 1-3%.
Embodiment 1
A kind of Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
PH adjusting agent
Surplus is DMF.
The particle diameter of carbon black is 3 μm, and function additive is click conifer antimildew disinfectant, and dispersant is polyacrylate, and the addition of pH adjusting agent is for regulating mill base pH to be 7.
The preparation method of Graphene modification mill base as above, comprises the following steps:
1. solvent and dispersant are added in blender, with 500 ~ 700r/min Rate Dispersion 15 minutes, obtain the first mixed solution;
2. function additive is added in the first mixed solution and mix, obtain the second mixed solution;
3. Graphene and carbon black are added the second mixed solution, obtain the pre-dispersed slurry of carbon black;
4. pre-dispersed for carbon black slurry is not less than 30 minutes with the Rate Dispersion of 1500 ~ 3000r/min, and in dispersion process, slowly adds pH value regulator control pH 7, obtain premixed carbon black;
5. premixed carbon black is ground, when its particle diameter reach≤0.2 μm time stop grinding, with the Rate Dispersion 15 minutes of 1500r/min, obtain initial carbon black;
6. quality testing, vacuum defoamation and after filtering and packaging are carried out to initial carbon black, obtain Graphene modification mill base.
Above-mentioned Graphene modification mill base is mixed with spinning solution in spinning process, carries out spinning, obtain colored textiles.
Far infrared the performance test results is: normal emittance 0.8, and antibacterial bacteriostatic performance test result is: be 50% to Escherichia coli, staphylococcus aureus antibacterial bacteriostatic rate.
Embodiment 2
A kind of Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
PH adjusting agent
Surplus is DMF.
The particle diameter of carbon black is 4 μm, and function additive is cellulose ether, and dispersant is polyoxyethylene ether, and the addition of pH adjusting agent is for regulating mill base pH to be 11.
Preparation method, with embodiment 1, removes and in dispersion process, slowly adds pH value regulator control pH 11.
Above-mentioned Graphene modification mill base is mixed with spinning solution in spinning process, carries out spinning, obtain colored textiles.
Far infrared the performance test results is: normal emittance 0.9, and antibacterial bacteriostatic performance test result is: be 98% to Escherichia coli, staphylococcus aureus antibacterial bacteriostatic rate.
Embodiment 3
A kind of Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
PH adjusting agent
Surplus is water.
The particle diameter of carbon black is 3 μm, and function additive is dodecyl benzyl dimethyl ammonium chloride, and dispersant is benzyl naphthalenesulfonate formaldehyde condensation compound, and the addition of pH adjusting agent is for regulating mill base pH to be 7.
Preparation method is with embodiment 1.
Above-mentioned Graphene modification mill base is mixed with spinning solution in spinning process, carries out spinning, obtain colored textiles.
Far infrared the performance test results is: normal emittance 0.89, and antibacterial bacteriostatic performance test result is: be 98% to Escherichia coli, staphylococcus aureus antibacterial bacteriostatic rate.
Embodiment 4
A kind of Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
PH adjusting agent
Surplus is water.
The particle diameter of carbon black is 3 μm, and function additive is dodecyl benzyl dimethyl ammonium chloride, and dispersant is benzyl naphthalenesulfonate formaldehyde condensation compound, and the addition of pH adjusting agent is for regulating mill base pH to be 7.
Preparation method is with embodiment 1.
Above-mentioned Graphene modification mill base is mixed with spinning solution in spinning process, carries out spinning, obtain colored textiles.
Far infrared the performance test results is: normal emittance 0.88, and antibacterial bacteriostatic performance test result is: be 95% to Escherichia coli, staphylococcus aureus antibacterial bacteriostatic rate.
Compared with embodiment 3, embodiment 4 optimizes the content of Graphene further, and function is suitable with interpolation 5% Graphene, but cost significantly reduces, and standing 2h has precipitation to produce.
Embodiment 5
All the other are identical with embodiment 4, and the particle diameter except carbon black is about 2 μm.
Above-mentioned Graphene modification mill base is added in spinning solution, carries out spinning, obtain colored textiles.
Compared with embodiment 4, embodiment 5 pairs of particle size carbon blacks are optimized, and dispersive property is more superior, leave standstill 2h and generate without precipitation.
Comparative example 1
All the other are with embodiment 4, and the content except Graphene is 0.01%.
Above-mentioned Graphene modification mill base is added in spinning solution, carries out spinning, obtain colored textiles.
Compared with embodiment 4, comparative example 1 added a small amount of Graphene, and far infrared the performance test results is normal emittance 0.78, antibacterial bacteriostatic performance test result is for being 10% to Escherichia coli, staphylococcus aureus antibacterial bacteriostatic rate.
Comparative example 2
All the other are with embodiment 4, and the content except Graphene is 7%.
Above-mentioned Graphene modification mill base is added in spinning solution, carries out spinning, obtain colored textiles.
Compared with embodiment 4, comparative example 2 added the Graphene of volume, and Graphene addition is too much, and cause dispersion uneven, sediment appears in standing 2h.
Comparative example 3
All the other are identical with embodiment 4, and the particle diameter except carbon black is 8 μm.
Above-mentioned Graphene modification mill base is added in spinning solution, carries out spinning, obtain colored textiles.
Compared with embodiment 4, comparative example 3 have selected the carbon black of Large stone, disperses uneven, leaves standstill 1h and occurs precipitation, spinning process blocking spinning head.
Comparative example 4
The Graphene of amount identical with embodiment 4 is added in spinning solution, carries out spinning, obtain colored textiles.
Graphene is added in mill base and can be more applicable for suitability for industrialized production, do not need all will join weaving liquid at every turn; And dispersion effect is comparatively outstanding, observed by color and luster, pigment is uniformly dispersed.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a Graphene modification mill base, it comprises following component by the percentage by weight that each component accounts for:
2. mill base as claimed in claim 1, it is characterized in that, the content of described Graphene is 0.1 ~ 3%;
Preferably, described Graphene is prepared by living beings;
Preferably, the content of described carbon black is 20-35%;
Preferably, the particle diameter of described carbon black is < 5 μm, is preferably less than 2 μm.
3. the mill base as described in one of claim 1-2, is characterized in that, the content of described function additive is 5 ~ 15%, is preferably 10 ~ 15%;
Preferably, described function additive is propylene glycol monomethyl ether, EGME, dimethyl sulfoxide (DMSO), dimethyl propylene glycol, glycerol, propylene glycol, ethylene glycol, polypropylene glycol, polyethylene glycol, dodecyl benzyl dimethyl ammonium chloride, cellulose ether, isothiazolinone, bohr ripple is many, the combination of any one or at least two kinds in click conifer antimildew disinfectant or defoamer, preferred propylene glycol monomethyl ether, EGME, dimethyl sulfoxide (DMSO), dimethyl propylene glycol, glycerol, propylene glycol, ethylene glycol, the combination of any one or at least two kinds in polypropylene glycol or polyethylene glycol,
Preferably, described defoamer is the combination of any one or at least two kinds in mineral oil antifoam agent, phosphate defoamer, fat hydrocarbon defoamer or silicone oil defoamer.
4. the mill base as described in one of claim 1-3, is characterized in that, the content of described dispersant is 5 ~ 15%;
Preferably, described dispersant is the mixture of any one or at least two kinds in ammonium polyacrylate salt, polyacrylic acid sodium salt, di-2-ethylhexylphosphine oxide first sodium naphthalene sulfonate, benzyl naphthalenesulfonate formaldehyde condensation compound, naphthalenesulfonic acid-formaldehyde condensate, sulfocarbolate formaldehyde condensation products, phenolic aldehyde polyoxyethylene ether, polyoxyethylene ether, derivative of fatty acid, polyacrylate, modified polyacrylate, alkyl sulfate or alkyl sulfonate compound;
Preferably, described solvent is that DMF is or/and deionized water.
5. the mill base as described in one of claim 1-4, is characterized in that, described mill base also comprises pH adjusting agent;
Preferably, described pH adjusting agent is NaOH, KOH, NH
3h
2o, CH
3cOOH, Co (NH
2)
2, HCON (CH
3)
2, 1-METHYLPYRROLIDONE, any one or at least two kinds in NOP or triethanolamine mixture;
Preferably, add pH adjusting agent to regulate pH to 7 ~ 11 of mill base, the pH preferably regulating mill base is 7;
Preferably, particle diameter≤0.2 μm of described mill base.
6. a preparation method for the Graphene modification mill base as described in one of claim 1-5, comprises the following steps:
(1) by Graphene, carbon black, function additive, dispersant, solvent and optionally pH adjusting agent mixing, premixed carbon black is obtained;
(2) premixed carbon black is ground, obtain Graphene modification mill base.
7. method as claimed in claim 6, it is characterized in that, step (1) obtains premixed carbon black and comprises the following steps:
A function additive adds in the mixed solution of solvent and dispersant by ();
B Graphene and carbon black add in the mixed solution that step (a) obtains by (), obtain the pre-dispersed slurry of carbon black;
C the pre-dispersed slurry of carbon black of gained in step (b) is not less than 30 minutes with the Rate Dispersion of 1500 ~ 3000r/min by (), and in dispersion process, slowly add pH value regulator control pH at 7-11, obtains premixed carbon black.
8. method as claimed in claims 6 or 7, is characterized in that, described in be ground to the combination of micro-any one or at least two kinds penetrated in pulverizing or horizontal grinding of ball milling, basket grinding, homogeneous;
Preferably, premixed carbon black is ground, stop grinding when its particle diameter reaches D90≤0.2 μm;
Preferably, also comprise after stopping grinding, with the Rate Dispersion at least 15 minutes of 1500r/min, obtain the step of initial carbon black;
Preferably, also comprise initial carbon black quality testing, vacuum defoamation and the step that filters and packages.
9. the method as described in one of claim 6-8, is characterized in that, comprises the following steps:
(1) solvent and dispersant are added in blender, with 500 ~ 700r/min Rate Dispersion 15 minutes, obtain the first mixed solution; Function additive is added in the first mixed solution and mix, obtain the second mixed solution; Graphene and carbon black are added the second mixed solution, obtains the pre-dispersed slurry of carbon black; Pre-dispersed for carbon black slurry is not less than 30 minutes with the Rate Dispersion of 1500 ~ 3000r/min, and in dispersion process, slowly adds pH value regulator control pH 7 ~ 11, obtain premixed carbon black;
(2) premixed carbon black is ground, when its particle diameter reach≤0.2 μm time stop grinding, with the Rate Dispersion 15 minutes of 1500r/min, obtain initial carbon black; Quality testing, vacuum defoamation and after filtering and packaging are carried out to initial carbon black, obtains Graphene modification mill base.
10. a purposes for the Graphene modification mill base as described in one of claim 1-5, carries out spinning and prepares colored textiles after it being mixed with spinning solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610021013.6A CN105543993B (en) | 2016-01-13 | 2016-01-13 | A kind of graphene is modified mill base, preparation method and its usage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610021013.6A CN105543993B (en) | 2016-01-13 | 2016-01-13 | A kind of graphene is modified mill base, preparation method and its usage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105543993A true CN105543993A (en) | 2016-05-04 |
| CN105543993B CN105543993B (en) | 2018-03-30 |
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| CN110277184A (en) * | 2019-05-29 | 2019-09-24 | 常熟理工学院 | A kind of graphene mill base and preparation method thereof and application in a fuel cell |
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| CN111155187A (en) * | 2020-01-19 | 2020-05-15 | 浙江纳美新材料股份有限公司 | Conductive black water-based color paste for coloring viscose stock solution and preparation method thereof |
| CN111607296A (en) * | 2020-06-02 | 2020-09-01 | 上海金狮化工有限公司 | Functional graphene modified water-based leather color paste and preparation method thereof |
| CN112791697A (en) * | 2020-12-16 | 2021-05-14 | 华南理工大学 | Elastic super-hydrophobic graphene gel sphere and preparation method and application thereof |
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| CN108047709A (en) * | 2017-12-29 | 2018-05-18 | 福建华彩新材料有限公司 | A kind of Graphene antibiosis master batch, fiber and preparation method thereof |
| CN110277184A (en) * | 2019-05-29 | 2019-09-24 | 常熟理工学院 | A kind of graphene mill base and preparation method thereof and application in a fuel cell |
| CN110373764A (en) * | 2019-06-26 | 2019-10-25 | 圣华盾防护科技股份有限公司 | A kind of antibacterial antistatic graphene viscose yarn and preparation method thereof |
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| CN110711070A (en) * | 2019-09-25 | 2020-01-21 | 张小伏 | Preparation method of far infrared graphene condom |
| CN111155187A (en) * | 2020-01-19 | 2020-05-15 | 浙江纳美新材料股份有限公司 | Conductive black water-based color paste for coloring viscose stock solution and preparation method thereof |
| CN111607296A (en) * | 2020-06-02 | 2020-09-01 | 上海金狮化工有限公司 | Functional graphene modified water-based leather color paste and preparation method thereof |
| CN112791697A (en) * | 2020-12-16 | 2021-05-14 | 华南理工大学 | Elastic super-hydrophobic graphene gel sphere and preparation method and application thereof |
| CN112791697B (en) * | 2020-12-16 | 2022-08-05 | 中山市华锌工材料科技有限公司 | Elastic super-hydrophobic graphene gel ball and preparation method and application thereof |
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