CN105131333A - Preparation method of carbon black fluid - Google Patents
Preparation method of carbon black fluid Download PDFInfo
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Abstract
The invention relates to a preparation method of carbon black fluid. The preparation method is characterized in that acidified carbon black aqueous dispersion and segmented copolymer aqueous dispersion are mixed, and the mixed liquor is dried, so as to obtain the carbon black fluid. According to the preparation method of the carbon black fluid, provided by the invention, the preparation process is simple, the reaction period is short, no organic solvent is used in the reaction process, and environmental pollution is avoided; besides, the carbon black fluid prepared by adopting the preparation method is uniform in particle size distribution, lower in the melting point when compared with that of carbon black fluid prepared by adopting other methods, has more excellent performance, and further has a good prospect in application of polymers.
Description
Technical field
The present invention relates to inorganic nanoparticle surface modification technology, specifically a kind of preparation method of carbon black fluid.
Background technology
Nanoparticle is by the less atom of number or molecular atom group or molecular group, and its surface atom is not only without long-range order but also without the amorphous layer of short-range order; And in particle heart portion, there is the atom of complete crystallization periodic arrangement.Due to this special construction of nanoparticle, make nano material have the characteristics such as special surface effects, volume effect, quantum size effect and macro quanta tunnel effect, and produce many physicochemical property different from Conventional solid thus.But because nano-particles size is very little, great surface energy easily makes it to reunite.After inorganic nano-particle is reunited, a lot of excellent performance of nano material can be destroyed.Therefore apply time must carry out surface treatment to inorganic nano-particle, by primary partical or comparatively small agglomerates stablize, stop reunite occur.
But in research in the past, nanoparticle all presents the state of solid when not containing solvent.And class fluid nanoparticle is by covalent linkage or ion-exchange long-chain organism in nanoparticle surface grafting, the class fluid of formation, under the condition of normal temperature and pressure, not containing any solvent, presents the similar fluid state of one-component.Nanometer class fluid is exactly collect the physics-chem characteristic of rice corpuscles and the rheological property system of fluid, and they have broad application prospects, such as; This solvent-free nanometer fluid is the same with solid nanoparticles, does not have solvent to environment: meanwhile, and nanometer class fluid provides a kind of novel method nanoparticle being processed into film and other functional form; Nanometer class fluid or novel emr fluid; In addition, the reaction medium that in class fluid, the space constraint of nanoparticle self and the physical and chemical performance of intrinsic thereof make this liquid can become novel.
In the prior art, Chinese patent CN200610124455.X, publication date on September 5th, 2006, denomination of invention is " solvent-free inorganic nano particle fluid and preparation method thereof ", and this invention utilizes organosilicon quaternary ammonium salt and polyoxyethylene sulfonic acid salt modified inorganic nano-particle to prepare similar nanofliuds.Chinese patent CN201210132099.1, publication date is on April 28th, 2012, denomination of invention is " having Ion nanometer material of fluid behavior and preparation method thereof under a kind of room temperature ", and this invention utilizes pyrrolidone hydrochloride and the sulfonate modified inorganic nano-particle of aliphatic alcohol polyethenoxy to obtain similar nanofliuds particulate material.Chinese patent CN201210044621.0, publication date is on August 1st, 2012, denomination of invention is " preparation method of a kind of novel core-shell-crown structure solvent-free nanometer class fluid ", and this invention obtains the nano-fluid with nucleocapsid structure equally by replacing amine modification with band sulfonic acid group coating materials and three after reduction reaction synthetics nano molybdenum disulfide particle.Above-mentioned research is all obtain nano-fluid by a series of grafting and substitution reaction, and reaction process is loaded down with trivial details, and reaction time is long.
Chinese patent CN103360801A, publication date on October 23rd, 2013, denomination of invention is " a kind of novel nano fluid and its preparation method and application ", this invention is by carrying out activation treatment with coupling agent to particle surface, by the reaction of epoxy-functional and ammonium salt, then obtains the surperficial nanofliuds with longer organic molecule chain through carrying out ion-exchange with polyoxyethylene.The method reaction process is simple, but reaction time is long, and employs volatile organic solvent in reaction process, easily causes environmental pollution, not environmentally.
The carboxyl (-COOH) that Zhang Xi etc. utilize the terminal hydroxy group (-OH) in amphipathic three block copolymer surperficial with functionalized multi-wall carbonnanotubes (MWNTs-COOH), hydrogen bond action between hydroxyl (-OH), or the voluble wrapping effect of amphipathic nature block polymer realizes the modification for multi-wall carbon nano-tube tube-surface, prepare multi-walled carbon nano-tubes/triblock copolymer (MWNTs-COOH/PPP) solvent-free nanometer fluid (Zhang Xi, Zheng Yaping, Lan Lan, Li Huayi, Yang Haicheng. the preparation of carbon nanotube/triblock polymer (PPP) solvent-free fluid and the impact [J] on Properties of Polypropylene. polymer material science and engineering, 2013, 04:155-159.) document does not relate to the preparation of carbon black/triblock copolymer solvent-free nanometer fluid.
In reaction process how with an organic solvent the method for current preparation solvent-free nanometer class fluid is more, but common method finally prepares nano-fluid by a series of grafting and substitution reaction, and feature is consuming time longer, and reaction time is long, and, be unfavorable for environmental protection.
Summary of the invention
For above-mentioned technology Problems existing, the object of the invention is to provide a kind of preparation method of carbon black fluid.For achieving the above object, the present invention is achieved by the following technical solutions:
A preparation method for carbon black fluid, described preparation method according to the following steps:
A. preparing particle diameter by acid oxidation is 15 ~ 30nm acidifying carbon black, then gets acidifying carbon black and deionized water that mass ratio is 1 ~ 4:800, by supersound process, obtains acidifying sooty water dispersion liquid.Ultrasonic power is 200W, ultrasonic time 1 ~ 2h;
B. segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 is dissolved in deionized water, pass through mechanical stirring, churning time 1 ~ 3h, the segmented copolymer aqueous solution of obtained mass concentration scope 5% ~ 30%, then the segmented copolymer aqueous solution is blended with the acidifying sooty water dispersion liquid obtained through a step, mechanical stirring 24h, obtain acidifying carbon black/segmented copolymer mixed dispersion liquid, finally by acidifying carbon black/segmented copolymer mixed dispersion liquid, be placed in vacuum-drying 36h, the mass ratio obtaining acidifying carbon black and segmented copolymer is 0.4 ~ 30:100, particle size range is the carbon black fluid of 20 ~ 50nm.
Owing to have employed above technical scheme, the preparation method of a kind of carbon black fluid of the present invention has the following advantages:
The present invention utilizes the hydrogen bond action formed between the carboxyl (-COOH) of amphipathic three block copolymer terminal hydroxy group (-OH) and acidifying carbon blacksurface, hydroxyl (-OH), or realize the modification for acidifying carbon blacksurface by the voluble wrapping effect of amphipathic nature block polymer, prepare carbon black fluid.The present invention prepares the method for carbon black solvent-free nanometer fluid, the method preparation process is simple, and reaction time is short, and in reaction process not with an organic solvent, do not pollute the environment, it is different from tradition and adopts a series of grafting and substitution reaction to prepare the method for nanometer class fluid.Carbon black fluid prepared by the present invention simultaneously, its size distribution is homogeneous, scope is 20 ~ 50nm, it is lower that fusing point compares carbon black fluid prepared by other method, its performance is more excellent, carbon black fluid prepared by the method, can not only toughen and intensify polymkeric substance and can as the conductive filler material of polymkeric substance, and its application prospect widely.
Embodiment
Below in conjunction with specific examples, the present invention is described in further detail.
The method with carbon black inorganic nano-particle for material, utilize the hydrogen bond action between the carboxyl (-COOH) on carbon black particle surface after terminal hydroxy group (-OH) in amphipathic three block copolymer and acid oxidase, hydroxyl (-OH), or the voluble wrapping effect of amphipathic nature block polymer realizes the modification for carbon blacksurface, prepares carbon black fluid.
A preparation method for carbon black fluid, described preparation method according to the following steps:
A. preparing particle diameter by acid oxidation is 15 ~ 30nm acidifying carbon black, then gets acidifying carbon black and deionized water that mass ratio is 1 ~ 4:800, by supersound process, obtains acidifying sooty water dispersion liquid.Ultrasonic power is 200W, ultrasonic time 1 ~ 2h;
B. segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 is dissolved in deionized water, pass through mechanical stirring, churning time 1 ~ 3h, the segmented copolymer aqueous solution of obtained mass concentration scope 5% ~ 30%, then the segmented copolymer aqueous solution is blended with the acidifying sooty water dispersion liquid obtained through a step, mechanical stirring 24h, obtain acidifying carbon black/segmented copolymer mixed dispersion liquid, finally by acidifying carbon black/segmented copolymer mixed dispersion liquid, be placed in vacuum-drying 36h, the mass ratio obtaining acidifying carbon black and segmented copolymer is 0.4 ~ 30:100, particle size range is the carbon black fluid of 20 ~ 50nm.
Specific embodiment
embodiment 1
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.05g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1h, obtained massfraction is the segmented copolymer aqueous solution of 5wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 5wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 2
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.05g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1h, obtained massfraction is the segmented copolymer aqueous solution of 10wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 10wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 3
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.05g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1.5h, obtained massfraction is the segmented copolymer aqueous solution of 15wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 15wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 4
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.1g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1h, obtained massfraction is the segmented copolymer aqueous solution of 10wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 10wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 5
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.1g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1.5h, obtained massfraction is the segmented copolymer aqueous solution of 15wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 15wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 6
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.1g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 2h, obtained massfraction is the segmented copolymer aqueous solution of 20wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 20wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 7
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.15g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1h, obtained massfraction is the segmented copolymer aqueous solution of 10wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 10wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 8
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.15g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1.5h, obtained massfraction is the segmented copolymer aqueous solution of 15wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 15wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 9
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.15g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 2h, obtained massfraction is the segmented copolymer aqueous solution of 20wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 20wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 10
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.15g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1.5h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 3h, obtained massfraction is the segmented copolymer aqueous solution of 25wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 25wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 11
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.2g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 2h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1h, obtained massfraction is the segmented copolymer aqueous solution of 10wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 10wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 12
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.2g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 2h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 1.5h, obtained massfraction is the segmented copolymer aqueous solution of 15wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 15wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 13
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.2g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 1h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 2h, obtained massfraction is the segmented copolymer aqueous solution of 20wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 20wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 14
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.2g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 2h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 3h, obtained massfraction is the segmented copolymer aqueous solution of 25wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 25wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
embodiment 14
The surface oxidation of 1 carbon black: get 5g carbon black, adds in the mixed acid solution (vitriol oil/concentrated nitric acid volume ratio is 3:1) of 100ml, in ultrasonic cleaner 70 DEG C of ultrasonic oxidation 10h; Afterwards with a large amount of distilled water diluting to solution in neutral, adopt the millipore filtration of φ 0.22 μm to carry out suction filtration to filtrate in neutral, the solid sample obtained be placed in vacuum drying oven, vacuum-drying 12h, obtain acidifying carbon black.
The preparation of 2 carbon black class fluids:
A. get acidifying carbon black dispersion that 0.2g prepared in step 1 in 40ml deionized water, by supersound process, obtain the aqueous dispersions of acidifying carbon black.Ultrasonic power is 200W, ultrasonic time 2h;
B. dissolved in deionized water by segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 (PEO-b-PPO-b-PEO), by mechanical stirring, churning time 3h, obtained massfraction is the segmented copolymer aqueous solution of 30wt%.Then be that the acidifying sooty water dispersion liquid that obtains in the segmented copolymer aqueous solution of 30wt% and a step is blended by massfraction, mechanical stirring 24h, obtain the mixed dispersion liquid of acidifying carbon black/segmented copolymer, finally by the mixed dispersion liquid of acidifying carbon black/segmented copolymer, be placed in vacuum-drying 36h, finally obtained carbon black fluid.
Claims (1)
1. a preparation method for carbon black fluid, is characterized in that: described preparation method according to the following steps:
A. preparing particle diameter by acid oxidation is 15 ~ 30nm acidifying carbon black, and then get acidifying carbon black and deionized water that mass ratio is 1 ~ 4:800, by supersound process, obtain acidifying sooty water dispersion liquid, ultrasonic power is 200W, ultrasonic time 1 ~ 2h;
B. segmented copolymer Pluronic F-127-polyphenylene oxide-Pluronic F-127 is dissolved in deionized water, pass through mechanical stirring, churning time 1 ~ 3h, the segmented copolymer aqueous solution of obtained mass concentration scope 5% ~ 30%, then the segmented copolymer aqueous solution is blended with the acidifying sooty water dispersion liquid obtained through a step, mechanical stirring 24h, obtain acidifying carbon black/segmented copolymer mixed dispersion liquid, finally by acidifying carbon black/segmented copolymer mixed dispersion liquid, be placed in vacuum-drying 36h, the mass ratio obtaining acidifying carbon black and segmented copolymer is 0.4 ~ 30:100, particle size range is the carbon black fluid of 20 ~ 50nm.
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