CN106634060A - Preparation method of oily self-dispersing nano carbon black - Google Patents
Preparation method of oily self-dispersing nano carbon black Download PDFInfo
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- CN106634060A CN106634060A CN201611166125.7A CN201611166125A CN106634060A CN 106634060 A CN106634060 A CN 106634060A CN 201611166125 A CN201611166125 A CN 201611166125A CN 106634060 A CN106634060 A CN 106634060A
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- carbon black
- oiliness
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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
- C09C3/06—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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a preparation method of oily self-dispersing nano carbon black and belongs to the field of fine chemical industry. A silane coupling agent containing carbon-carbon double bonds is grafted on the surface of carbon black, polymerizable groups of the silane coupling agent are utilized to copolymerize with other oily monomers, the surfaces of carbon black particles are coated with a layer of polymer having both dispersing and stabilizing effects, and then the objective of self-dispersing in oily solvents is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of oiliness self-dispersing nano carbon black, belongs to field of fine chemical.
Background technology
Carbon black is widely used in the numerous areas such as rubber, plastics, coating as a kind of important colouring agent, but due to carbon black
Particle size is little, specific surface area is big, easily reunite etc. characteristic, it is difficult to be stably dispersed in oleaginous system, these defects are limited
Carbon black performance gives full play to, it has also become a great problem of carbon black application.Therefore, strengthen the lipophile of carbon black, raising carbon black to exist
Dispersion stabilization in oil-based solvent has become current study hotspot.
Oiliness self-dispersing charcoal blacks are a kind of new coloured materials for developing in recent years, with convenient transportation, using letter
Single the features such as, the extensive concern of people is obtained.At present, preparing the method for lipophile carbon black mainly has：(1) assist in dispersant
Lower grinding distribution, the method process is simple, is easy to industrialization, such as：Cui Ying etc. is with ionic fatty alcohol ether microcosmic salt and nonionic silicon
Alkane coupling agent has successfully disperseed polyacrylonitrile-based carbon fibre as dispersant, but because the dispersant for adding is by physical action
There is the phenomenon of absorption and De contamination in absorption, and the presence of De contamination behavior can cause carbon black particle to gather again in matrix surface
Collection.(2) coating modification, typically using carbon black as the capsule heart, oil-based polymer is wall material to this method, is gathered by phase separation, surface
Oil-based polymer is deposited on carbon blacksurface by the method close, being spray-dried, and forms microcapsules, allow carbon black particle it is stable point
In being dispersed in oil-based solvent.Such as：Patent CN101418137 discloses a kind of in-situ polymerization, and to prepare ultrafine organic paint/polymer multiple
The method for closing powder, success is in organic pigment or carbon blacksurface cladding one layer of polymeric so as to divide well in specific solvent
Scattered stability.But such method is mostly for mill base and the most particle diameter of modified carbon black of preparation is larger, not in nanometer
In the range of.(3) graft modification, the graft modification of carbon blacksurface is the oiliness polymer chain in carbon blacksurface grafting, and by one
End is firmly bonded to carbon blacksurface, and the other end stretches in a solvent to provide enough repulsion and prevent to be reassembled between particle
Reach readily dispersible purpose.Such as level land Ji Fu by being grafted azo group or peroxide ester group in carbon blacksurface, in the feelings of heating
Cause oil-soluble ethylene base monomer to be polymerized under condition, obtain the modified carbon black with core shell structure, have in oil-based solvent
Good dispersive property.But this method is harsh due to grafting conditions, initiation temperature is high, and efficiency of initiation is low to be caused coating completely
Entirely, particle diameter larger (mostly in micron level)；In addition these modifying process are carried out in some poisonous and hazardous solvents mostly, right
Environment has certain damaging effect.
The content of the invention
The purpose of the present invention is：Exploitation nano carbon black with good self-dispersing function in oil-based system so as to meet
Requirement of the fiber such as terylene, PLA original liquid coloring to carbon black, so as to overcome dispersion in because adding other materials, such as disperse
Agent, wetting agent etc. and cause the impaired phenomenon of fibre structure, mechanical property and apparent form, overcome transportation environment to make colouring agent
With the impact of 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, deionized water is subsequently adding,
And the pH value of regulation system；Then, reaction system is transferred in reactor, uniform temperature reaction a period of time；Add oiliness
Comonomer, is warming up to uniform temperature, starts that initiator is added dropwise and the reaction time is controlled, and Jing high speed centrifugations, washing, drying will
Dried carbon black powder is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain oiliness self-dispersing 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 1～10% to Oxygen in Liquid agent mass fraction, oxidizing temperature 50
～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 0.1～50% to the mass-dispersion of oxidation modification carbon black, and addition deionized water is to the mass fraction of alcoholic solvent
0.1～90%, pH value is adjusted between 2～11, first step reaction temperature is 20～80 DEG C in reactor, and the reaction time is 0.5
～30h, adds oiliness comonomer to be 50～200% to the mass fraction of oxidation modification carbon black, and copolymerization temperature is 50～90 DEG C,
Initiator is 0.5～15% to monomer mass fraction, reacts 0.5～20h.
In one embodiment of the invention, mass fraction of the carbon black in alcoholic solvent is 1～10%, silane coupler
It is 10～50% to the mass-dispersion of oxidation modification carbon black, adds deionized water to be 50～90% to the mass fraction of alcoholic solvent,
PH value is adjusted between 3～9, first step reaction temperature is 40～80 DEG C in reactor, the reaction time is 10～24h, adds oil
Property comonomer be 100～200% to the mass fraction of oxidation modification carbon black, copolymerization temperature is 60～90 DEG C, and initiator is to list
Weight fraction is 0.5～5%, reacts 6～10h.
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 pulverizer.
In one embodiment of the invention, the pH adjusting agent be NaOH, sodium acid carbonate, ammoniacal liquor, triethylamine,
One kind in triethanolamine.
In one embodiment of the invention, the oiliness comonomer be methyl acrylate, methyl methacrylate,
Ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, lauryl alcohol ester, acrylic acid hydroxypropyl
One kind in ester, hydroxy propyl methacrylate, glycidyl acrylate, methacrylic acid urea groups ester.
In one embodiment of the invention, the initiator is azodiisobutyronitrile, ABVN, peroxidating
Diisopropylbenzene (DIPB), di-tert-butyl peroxide, dibenzoyl peroxide, dilauroyl peroxide, DCPD or mistake
Aoxidize two diisopropyl carbonates.
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.The silane coupler containing carbon-carbon double bond is grafted in carbon blacksurface,
And with other oiliness monomer copolymerizations, carbon blacksurface coat one layer have disperse and stable double action polymer, Jing centrifugations,
Washing, drying prepare oiliness self-dispersing nano carbon black.The method has simple production process, easy to operate, the features such as environmentally friendly；
Ensure that carbon black particle is in nanometer range in whole process using the dispersive property of silane coupler；Adjusting process can be passed through
The particle diameter and polymer thickness of condition control compound particle.Modified carbon black prepared by the present invention particle diameter in oil medium is little, grain
Footpath narrowly distributing, and with excellent shelf-stability.Also there is good self-dispersing energy in acetone soln, it is in acetone soln
In particle diameter in 190～230nm or so, PDI is 0.1～0.2 or so.
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 0.5g methyl methacrylates, be warming up to
60 DEG C, start that the initiator azodiisobutyronitrile for weighing monomer 0.5% is added dropwise, react 0.5h, Jing high speed centrifugations, washing is dried,
Dried carbon black powder is ground with pulverizer, and is filtered with 200 mesh filter screens, you can obtain oiliness self-dispersing Nano carbon
Mineral black.
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 4g silane coupler KH570 to be dissolved in 60g ethanol solutions, add 8g 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 EMAs are added, it is warming up to 75
DEG C, start that the initiator ABVN 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 oiliness self-dispersing nano carbon black face
Material.
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.Weigh 2.5g
Silane coupling A 151 is dissolved in 50g ethanol solutions, adds 5g oxidation modification carbon blacks, and Jing ultrasonic cell disruptors are by carbon black
Nano particle is dispersed into, the deionized water of 25g is subsequently adding, and is turned reaction system to 8.5 with the pH value of ammoniacal liquor regulation system
In moving on to reactor, 24h is reacted at 40 DEG C, add 10g butyl methacrylates, be warming up to 75 DEG C, start to be added dropwise to monomer
5% initiator azodiisobutyronitrile is weighed, 10h, Jing high speed centrifugations, washing, drying, by dried carbon black powder powder is reacted
Broken machine grinds, and is filtered with 200 mesh filter screens, you can obtain oiliness self-dispersing nano carbon black pigment.
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 80g methyl methacrylates to be warming up to 90 DEG C, started
Dropwise addition weighs 5% initiator ABVN to monomer, reacts 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 oiliness self-dispersing nano carbon black pigment.
The quality parameter of each embodiment of table 1 gained oiliness self-dispersing nano carbon black pigment
| Particle diameter (nm) | Particle diameter distribution | Shelf-stability (my god) | |
| Embodiment 1 | 250 | 0.164 | 39 |
| Embodiment 2 | 173 | 0.131 | 41 |
| Embodiment 3 | 178 | 0.124 | 43 |
| Embodiment 4 | 170 | 0.112 | 42 |
Note：Particle diameter, particle diameter distribution adopt Nanosizer ZS90 (Malven Instruments Ltd) determine (solvent for
Acetone)；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 oiliness 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
Thermotonus is for a period of time；Oiliness comonomer is added, 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 oiliness 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 0.1～50% to the mass-dispersion of oxidation modification carbon black, adds deionized water to alcoholic solvent
Mass fraction be 0.1～90%, adjust pH value between 2～11, in reactor first step reaction temperature be 20～80 DEG C, instead
It is 0.5～30h between seasonable, adds oiliness comonomer to be 50～200% 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 and 2, it is characterised in that the carbon black is furnace black, channel black, crack it is black in one
Kind.
5. according to the arbitrary described method of Claims 1 to 4, it is characterised in that the Oxygen in Liquid agent is salpeter solution, peroxide
In changing hydrogen solution, saturation ammonium persulfate solution, perchloric acid, aqueous sodium hypochlorite solution, isocyanates solution, liquor potassic permanganate
It is a kind of.
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. according to the arbitrary described method of claim 1～6, it is characterised in that described alcoholic solvent be methyl alcohol, ethanol, propyl alcohol,
One kind in butanol, isopropanol, ethylene glycol, glycol monoethyl ether.
8. method according to claim 1, it is characterised in that the pH adjusting agent is NaOH, sodium acid carbonate, ammonia
One kind in water, triethylamine, triethanolamine.
9. according to the arbitrary described method of claim 1～8, it is characterised in that the oiliness comonomer be methyl acrylate,
Methyl methacrylate, ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, lauryl
One kind in alcohol ester, hydroxypropyl acrylate, hydroxy propyl methacrylate, glycidyl acrylate, methacrylic acid urea groups ester.
10. the oiliness self-dispersing nano carbon black for being prepared according to the arbitrary described method of claim 1～9.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084744A (en) * | 2017-12-22 | 2018-05-29 | 江南大学 | A kind of method that self-dispersing nano carbon black is prepared based on sulfydryl-alkene click-reaction |
| 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 |
| CN108841208A (en) * | 2018-05-28 | 2018-11-20 | 西安工程大学 | A method of carbon black is modified using POLYPROPYLENE GLYCOL and eliminates carbon black reunion |
| CN108864774A (en) * | 2018-07-20 | 2018-11-23 | 江南大学 | A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process |
| CN110129915A (en) * | 2019-05-28 | 2019-08-16 | 江南大学 | A kind of method that original liquid coloring prepares black acid fiber by polylactic |
| CN115717001A (en) * | 2022-11-21 | 2023-02-28 | 桂林电子科技大学 | Phosphorus-silicon acid coated carbon black and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084744A (en) * | 2017-12-22 | 2018-05-29 | 江南大学 | A kind of method that self-dispersing nano carbon black is prepared based on sulfydryl-alkene click-reaction |
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| CN108841208A (en) * | 2018-05-28 | 2018-11-20 | 西安工程大学 | A method of carbon black is modified using POLYPROPYLENE GLYCOL and eliminates carbon black reunion |
| CN108864774A (en) * | 2018-07-20 | 2018-11-23 | 江南大学 | A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process |
| CN110129915A (en) * | 2019-05-28 | 2019-08-16 | 江南大学 | A kind of method that original liquid coloring prepares black acid fiber by polylactic |
| CN115717001A (en) * | 2022-11-21 | 2023-02-28 | 桂林电子科技大学 | Phosphorus-silicon acid coated carbon black and preparation method and application thereof |
| CN115717001B (en) * | 2022-11-21 | 2024-02-06 | 桂林电子科技大学 | Phosphosilicic acid coated carbon black and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN106634060B (en) | 2018-07-03 |
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