CN106634059A - Preparation method of aqueous self-dispersing nanometer carbon black - Google Patents
Preparation method of aqueous self-dispersing nanometer carbon black Download PDFInfo
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- CN106634059A CN106634059A CN201611166095.XA CN201611166095A CN106634059A CN 106634059 A CN106634059 A CN 106634059A CN 201611166095 A CN201611166095 A CN 201611166095A CN 106634059 A CN106634059 A CN 106634059A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Abstract
The invention discloses a preparation method of aqueous self-dispersing nanometer carbon black, and belongs to the field of fine chemical engineering. Silane coupling agents containing carbon-carbon double bonds are grafted on the surface of carbon black; polymerizable groups of the silane coupling agents are used for being copolymerized with other aqueous monomers; a layer of polymers with duplex effects of dispersion and stabilization coats the surface of the carbon black particles, so that the goal of self dispersion in an aqueous solvent is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of aqueous self-dispersing nano carbon black, belongs to field of fine chemical.
Background technology
With the enhancing of countries in the world environmental consciousness, this not only save energy of coating and ink of water-based system but also protection ring
The product in border increasingly receives welcome.Carbon black has excellent coloring, weatherability and chemical stability, and abundance, valency
Lattice are cheap, are one of important colouring agents, but due to characteristics such as carbon black particle granularity is little, specific surface area big, easy reunions, it is difficult to surely
Surely it is dispersed in water-based system, these defects limit giving full play to for carbon black performance, it has also become a great problem of carbon black application.
Therefore, strengthen the hydrophily of carbon black, improve the focus that dispersion stabilization of the carbon black in aqueous solvent has become research.
Aqueous self-dispersing carbon black is a kind of new coloured material for developing in recent years, with convenient transportation, using simple etc.
Feature, has obtained the extensive concern of people.At present, preparing self-dispersing carbon black method mainly has：(1) grind under dispersant assistance
Dispersion, the method process is simple is easy to industrialization.Such as：Wang Shirong etc. is disperseed by synthesizing styrene and acrylic copolymer pigment
Agent so that the dispersion that pigment can be stable in water-based system, however, because the dispersant for adding is existed by physical action absorption
Carbon blacksurface, the phenomenon that there is absorption and De contamination, and the presence of De contamination behavior can cause carbon black particle to reassemble.(2)
Oxidation modification, by chemically or physically method oxidation processes are carried out to carbon blacksurface, increase carbon blacksurface acidity oxy radical (such as
Carboxyl, hydroxyl) content strengthening its dispersive property in aqueous solvent.Such as：Yang Xinyu et al. utilizes Oxygen in Liquid agent nitre
Acid carries out oxidation processes to carbon blacksurface, is prepared for the nano carbon black with self-dispersing function.But due to the carboxyl, the hydroxyl that introduce
The lazy weight of base is more than enough, and strand falls short of and the relatively low group of these degree of ionization is not enough to provide enough in a solvent
Repulsion is reaching the purpose of stable dispersion.(3) coating modification, this method is typically using carbon black as the capsule heart, water-soluble polymer
For wall material, polymer deposits in carbon blacksurface, are formed by microcapsules by phase separation, surface aggregate, the method being spray-dried.
Such as：Patent CN102532939A discloses one kind and adopts hydrophile copolymers, and organic pigment is coated by spray drying process
Modified, the organic pigment after cladding has good self-dispersing energy in water phase.But the micro- glue of pigment prepared by this method
Capsule particle diameter is larger, mostly not in nanometer range.(4) graft modification, the graft modification of carbon blacksurface is in carbon blacksurface grafting
Upper polymer chain, and carbon blacksurface is firmly bonded to, extend in and provide in water between enough repulsion prevention particles again
Assemble to reach readily dispersible purpose.Such as level land Ji Fu is being added by being grafted azo group or peroxide ester group in carbon blacksurface
Cause water-soluble vinyl monomer to be polymerized in the case of heat, the modified carbon black with core shell structure is obtained, in aqueous solvent
In have good dispersive property.But this method is harsh due to grafting conditions, initiation temperature is high, and efficiency of initiation is low to cause bag
Cover not exclusively, particle diameter larger (mostly in micron level).Other these modifying process are mostly in some poisonous and hazardous solvents
Carry out, there is certain damaging effect to environment.
The content of the invention
The purpose of the present invention is：Exploitation divides certainly in aqueous phase system, NMMO dicyandiamide solutions, polyelectrolyte system with good
The nano carbon black of scattered function so as to meet viscose rayon, Lyocell fiber and acrylic fibers NaSCN system original liquid colorings to carbon black
Require, so as to overcome dispersion in because add other materials, such as dispersant, wetting agent and cause fibre structure, mechanical property
The phenomenon being damaged with apparent form, overcomes impact of the transportation environment to colouring agent performance.
Technical scheme：First carbon blacksurface is processed with Oxygen in Liquid agent, obtain oxidation modification carbon black, then
Silane coupler alcoholic solution is added, equipment is dispersed through by oxidation modification carbon black dispersion into nano particle, is subsequently adding a certain amount of
Deionized water, and the pH value of regulation system；Then reaction system is transferred in reactor, when reacting one section under uniform temperature
Between, aqueous comonomer is added, uniform temperature is warming up to, start that initiator is added dropwise and the reaction time is controlled, Jing high speed centrifugations, wash
Wash, dry, dried carbon black powder is ground with pulverizer, and with 200 mesh filter screens filter, you can obtain it is aqueous from point
Scattered nano carbon black pigment.
In one embodiment of the invention, carbon black is 0.1～20% to Oxygen in Liquid agent mass fraction, oxidizing temperature
20～100 DEG C, 0.5～10h of time.
In one embodiment of the invention, carbon black is 0.1～10% to Oxygen in Liquid agent mass fraction, oxidizing temperature
20～60 DEG C, 0.5～2h of time.
In one embodiment of the invention, mass fraction of the oxidation modification carbon black in alcoholic solvent is 1～40%, silicon
Alkane coupling agent is 0.1～100% to the mass fraction of oxidation modification carbon black, and addition deionized water is to the mass fraction of alcoholic solvent
10～90%, adjust pH value between 3～11, in reactor first step reaction temperature be 20～80 DEG C, the reaction time be 0.5～
30h, adds aqueous comonomer to be 25～500% to the mass fraction of oxidation modification carbon black, and copolymerization temperature is 50～90 DEG C, is drawn
It is 0.5～15% that agent is sent out to monomer mass fraction, reacts 0.5～20h.
In one embodiment of the invention, mass fraction of the oxidation modification carbon black in alcoholic solvent is 1～10%, silicon
Alkane coupling agent is 0.1～50% to the mass fraction of oxidation modification carbon black, and addition deionized water is to the mass fraction of alcoholic solvent
10～50%, adjust pH value between 3～9, in reactor first step reaction temperature be 40～80 DEG C, the reaction time be 20～
30h, adds aqueous comonomer to be 25～200% to the mass fraction of oxidation modification carbon black, and copolymerization temperature is 50～90 DEG C, is drawn
It is 0.5～5% that agent is sent out to monomer mass fraction, reacts 5～20h.
In one embodiment of the invention, the carbon black be furnace black, channel black, crack it is black in one kind.
In one embodiment of the invention, the Oxygen in Liquid agent is salpeter solution, hydrogenperoxide steam generator, saturation mistake
One kind in ammonium sulfate, perchloric acid, aqueous sodium hypochlorite solution, isocyanates solution, liquor potassic permanganate.
In one embodiment of the invention, described silane coupler is in KH-570, A171, KH-A172, A151
One kind.
In one embodiment of the invention, described alcoholic solvent is methyl alcohol, ethanol, propyl alcohol, butanol, isopropanol, second
One kind in glycol, glycol monoethyl ether
In one embodiment of the invention, the dispersing apparatus are high speed dispersor, emulsifying agent, sand mill, ultrasound
One kind in ripple cell disruptor.
In one embodiment of the invention, the pH adjusting agent is hydrochloric acid, acetic acid NaOH, sodium acid carbonate, ammonia
One kind in water, triethylamine, triethanolamine.
In one embodiment of the invention, described aqueous comonomer is acrylic acid, methacrylic acid, clothing health
Acid, acrylamide, sodium p styrene sulfonate, polymerizable dispersant DNS86, ANPS, AHPS, HMPS, R303, SAS, HPMAS, T-
100th, one kind in T-70, T-75.
In one embodiment of the invention, initiator is that potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, azo two are different
One kind in Butyl Amidine HCl salt, azo diisopropylamidinateand oxazoline hydrochloride.
Beneficial effects of the present invention：Silane coupler not only to carbon black has good dispersive property in alcoholic solution, and
Can and carbon blacksurface hydroxyl occur chemical bond combination, carbon blacksurface be grafted the silane coupler containing carbon-carbon double bond,
And with other water-soluble monomer copolymerization, carbon blacksurface coat one layer have disperse and stable double action polymer, Jing from
The heart, washing, drying prepare oiliness self-dispersing nano carbon black.The inventive method has simple production process, easy to operate, to environment friend
The features such as good；Ensure that carbon black particle is in nanometer range in whole process using the dispersive property of silane coupler；By adjusting
The particle diameter and polymer thickness of whole process regulation compound particle；In an aqueous medium particle diameter is little for the modified carbon black of preparation, grain
Footpath narrowly distributing, and with excellent shelf-stability.
Specific embodiment
Embodiment 1：
Process 0.5h is carried out to 0.6g carbon blacks at 20 DEG C with the salpeter solution (concentration is 30%) of 60g, oxidation is obtained and is changed
The carbon black of property.Weigh 0.1g silane coupling As 171 to be dissolved in 100g ethanol solutions, add 1g oxidation modification carbon blacks, Jing is ultrasonic
Carbon black dispersion into nano particle, is subsequently adding the deionized water of 10g by ripple cell disruptor, and with the pH value of ammoniacal liquor regulation system
To 8.5, reaction system is transferred in reactor, 0.5h is reacted at 20 DEG C, add 5g polymerizable dispersant A HPS, be warming up to
60 DEG C, start that the initiator ammonium persulfate for weighing monomer 0.5% is added dropwise, react 0.5h, Jing high speed centrifugations, washing, drying will be done
Carbon black powder after dry is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain aqueous self-dispersing nano carbon black face
Material.
Embodiment 2：
Process 2h is carried out to 4g carbon blacks at 60 DEG C with the hydrogenperoxide steam generator (concentration is 30%) of 40g, oxidation is obtained and is changed
The carbon black of property.Weigh 5g silane coupler KH570 to be dissolved in 60g ethanol solutions, add 5g oxidation modification carbon blacks, Jing ultrasonic waves
Carbon black dispersion into nano particle, is subsequently adding the deionized water of 30g by cell disruptor, and with the pH value of acetic acid regulation system extremely
3.5, reaction system is transferred in reactor, 24h is reacted at by 40 DEG C, 10g sodium p styrene sulfonates are added, it is warming up to 75
DEG C, start that the initiator ammonium persulfate for weighing monomer 5% is added dropwise, 6h is reacted, Jing high speed centrifugations, washing is dried, will be dried
Carbon black powder is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain aqueous self-dispersing nano carbon black pigment.
Embodiment 3：
Process 2h is carried out to 4g carbon blacks at 50 DEG C with 40g perchloric acid solutions, the carbon black of oxidation modification is obtained, is aoxidized
Modified carbon black.Weigh 2.5g silane coupling As 151 to be dissolved in 50g ethanol solutions, add 5g oxidation modification carbon blacks, Jing to surpass
Carbon black dispersion into nano particle, is subsequently adding the deionized water of 25g by sound wave cell disruptor, and with the pH of ammoniacal liquor regulation system
It is worth to 8.5, reaction system is transferred in reactor, 24h is reacted at 40 DEG C, add 5g polymerizable dispersant A NPS, heats up
To 75 DEG C, start that the initiator ammonium persulfate for weighing monomer 5% is added dropwise, react 6h, Jing high speed centrifugations, washing, drying, by drying
Carbon black powder afterwards is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain aqueous self-dispersing nano carbon black face
Material.
Embodiment 4：
Process 10h is carried out to 8g carbon blacks at 100 DEG C with 40g saturations ammonium persulfate solution, the carbon black of oxidation modification is obtained.
Weigh 20g silane coupler KH-A172 to be dissolved in 100g ethanol solutions, add 40g oxidation modification carbon blacks, Jing supersonic cells
Carbon black dispersion into nano particle, is subsequently adding the deionized water of 90g by pulverizer, and with the pH value of acetic acid regulation system to 3.5,
Reaction system is transferred in reactor, 30h is reacted at 80 DEG C, add 10g polymerizable dispersant DNS86, be warming up to 90 DEG C,
Start that the initiator potassium persulfate for weighing monomer 5% is added dropwise, react 20h, Jing high speed centrifugations, washing, drying, by dried charcoal
Black powder is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain aqueous self-dispersing nano carbon black pigment.
The quality parameter of the aqueous self-dispersing nano carbon black pigment of each embodiment of table 1 gained
| Particle diameter (nm) | Particle diameter distribution | Shelf-stability (my god) | |
| Embodiment 1 | 220 | 0.145 | 40 |
| Embodiment 2 | 190 | 0.131 | 42 |
| Embodiment 3 | 178 | 0.124 | 45 |
| Embodiment 4 | 170 | 0.112 | 46 |
Note：Particle diameter, particle diameter distribution adopt Nanosizer ZS90 (Malven Instruments Ltd) determine (solvent for
Water)；Shelf-stability is determined by the number of days that obvious sediment does not occur in beaker bottom.
Although the present invention is disclosed as above with preferred embodiment, it is not limited to the present invention, any to be familiar with this skill
The people of art, without departing from the spirit and scope of the present invention, can do various changes and modification, therefore the protection model of the present invention
Enclosing should be by being defined that claims are defined.
Claims (10)
1. a kind of method for preparing aqueous self-dispersing nano carbon black, it is characterised in that first carbon blacksurface is entered with Oxygen in Liquid agent
Row process, obtain oxidation modification carbon black, add silane coupler alcoholic solution, be dispersed through equipment by oxidation modification carbon black dispersion into
Nano particle, is subsequently adding deionized water, and the pH value of regulation system；Then reaction system is transferred in reactor, necessarily
At a temperature of reaction a period of time, add aqueous comonomer, uniform temperature is warming up to, when starting that initiator is added dropwise and reaction is controlled
Between, dried carbon black powder is crushed, filtered, you can obtains aqueous self-dispersing Nano carbon by Jing high speed centrifugations, washing, drying
Mineral black.
2. method according to claim 1, it is characterised in that carbon black is 0.1～20% to Oxygen in Liquid agent mass fraction,
20～100 DEG C of oxidizing temperature, 0.5～10h of oxidization time.
3. method according to claim 1 and 2, it is characterised in that mass fraction of the oxidation modification carbon black in alcoholic solvent
For 1～40%, silane coupler is 0.1～100% to the mass fraction of oxidation modification carbon black, adds deionized water to alcoholic solvent
Mass fraction be 10～90%, adjust pH value between 3～11, in reactor first step reaction temperature be 20～80 DEG C, instead
It is 0.5～30h between seasonable, adds aqueous comonomer to be 25～500% to the mass fraction of oxidation modification carbon black, copolymerization temperature
For 50～90 DEG C, initiator is 0.5～15% to monomer mass fraction, reacts 0.5～20h.
4. method according to claim 1, it is characterised in that the carbon black is furnace black, channel black, crack it is black in one kind.
5. method according to claim 1, it is characterised in that the Oxygen in Liquid agent is that salpeter solution, hydrogen peroxide are molten
One kind in liquid, saturation ammonium persulfate solution, perchloric acid, aqueous sodium hypochlorite solution, isocyanates solution, liquor potassic permanganate.
6. method according to claim 1, it is characterised in that described silane coupler is KH-570, A171, KH-
One kind in A172, A151.
7. method according to claim 1, it is characterised in that described alcoholic solvent is methyl alcohol, ethanol, propyl alcohol, butanol, different
One kind in propyl alcohol, ethylene glycol, glycol monoethyl ether.
8. method according to claim 1, it is characterised in that the pH adjusting agent is hydrochloric acid, acetic acid NaOH, carbonic acid
One kind in hydrogen sodium, ammoniacal liquor, triethylamine, triethanolamine.
9. method according to claim 1, it is characterised in that described aqueous comonomer is acrylic acid, metering system
Acid, itaconic acid, acrylamide, sodium p styrene sulfonate, polymerizable dispersant DNS86, ANPS, AHPS, HMPS, R303, SAS,
One kind in HPMAS, T-100, T-70, T-75.
10. the aqueous self-dispersing nano carbon black for being prepared according to the arbitrary methods described of claim 1～9.
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| CN108165054A (en) * | 2017-12-27 | 2018-06-15 | 南京工业大学 | A kind of preparation method of cation carbon black |
| CN108624090A (en) * | 2018-05-28 | 2018-10-09 | 西安工程大学 | A method of carbon black is modified using polyvinyl alcohol and eliminates carbon black reunion |
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