CN109240051A - A kind of ceramics carbon dust and preparation method thereof - Google Patents
A kind of ceramics carbon dust and preparation method thereof Download PDFInfo
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- CN109240051A CN109240051A CN201810954167.XA CN201810954167A CN109240051A CN 109240051 A CN109240051 A CN 109240051A CN 201810954167 A CN201810954167 A CN 201810954167A CN 109240051 A CN109240051 A CN 109240051A
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- Prior art keywords
- carbon dust
- wax
- charge control
- control agent
- dispersion liquid
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0802—Preparation methods
- G03G9/0804—Preparation methods whereby the components are brought together in a liquid dispersing medium
- G03G9/0806—Preparation methods whereby the components are brought together in a liquid dispersing medium whereby chemical synthesis of at least one of the toner components takes place
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/087—Binders for toner particles
- G03G9/08784—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775
- G03G9/08797—Macromolecular material not specially provided for in a single one of groups G03G9/08702 - G03G9/08775 characterised by their physical properties, e.g. viscosity, solubility, melting temperature, softening temperature, glass transition temperature
Abstract
The invention discloses a kind of ceramic carbon dusts and preparation method thereof, and ceramic carbon dust includes following component by weight: 15-30 parts of resin；60-80 parts of pigment；0.5-5 parts of charge control agent；0.5-5 parts of wax；0.1-4 parts of external additive；Preparation method is comprising steps of stock: preparing the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent；The mixed dispersion liquid of dispersible pigment dispersion, wax and charge control agent is using surfactant as dispersion liquid；Reaction: the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent is reacted under conditions of temperature is 40-55 DEG C, external additive is added after then cooling, filtering, drying, obtains ceramic carbon dust；Ceramic carbon dust has intact particle shape, relatively narrow particle diameter distribution and preferable mobility, can meet ceramic carbon dust transferring rate height, the high requirement of image density.
Description
Technical field
The present invention relates to a kind of ceramic carbon dusts and preparation method thereof, belong to printing material technical field.
Background technique
In ceramic industry, the floral designs of ceramic surface generally use manual drawing or the method for silk-screen printing to realize, so
And since manual drawing speed is slow, low efficiency, and be limited to the skill of mapper, floral designs are coarse, exquisite degree by
Limit, intolerant to seeing.Nowadays, silk-screen printing may be implemented to produce in enormous quantities, it is well known that can pass through silk-screen printing and ceramic paint ink
Pattern is printed upon on water-transfer printing paper by water, is then transferred in ceramic tile again, on glassware, or ceramic ink is directly printed upon
On wet ceramics, glassware, then by firing pattern is fixed, the high added values quotient such as personalized porcelain, ceramic tile, glass is made
Product, the decoration as family, hotel etc..However, silk-screen printing needs to prepare independent silk screen for each color, and use ceramics
Ink needs to reserve a drying time, while can also easily cause environmental pollution with the volatilization of solvent.
The main component of ceramic paint ink is ceramic carbon dust, ceramic carbon dust is produced using conventional physical method, due to ceramics
Pigment ratio is great, it is not easy to be uniformly dispersed in resin material, carbon dust electrification is uneven, so that carbon dust transferring rate is low, makes
Low at image density, image effect is bad.
Summary of the invention
For overcome the deficiencies in the prior art, the first purpose of this invention is to provide a kind of ceramic carbon dust, ceramic carbon
Powder has intact particle shape, relatively narrow particle diameter distribution and preferable mobility, can meet ceramic carbon dust transferring rate height, image density
High requirement.
Second object of the present invention is to provide a kind of preparation method of above-mentioned ceramic carbon dust, and the preparation method is in liquid phase
Middle progress, is conducive to that ceramic carbon meal component is uniform, carried charge is uniform
Realize that the first purpose of this invention can reach by adopting the following technical scheme that: a kind of ceramics carbon dust, including
Following component by weight:
Further, including following component by weight:
Further, resin includes acrylic resin and styrene resin with carboxyl functional group.
Further, the raw material for preparing resin includes following component by weight:
Further, resin is prepared by polymerization reaction；The reaction temperature of polymerization reaction is 55-90 DEG C, stirring speed
Degree is 150-900rpm.
Further, the fusing point of wax is 65-155 DEG C.
Further, external additive be silica of the surface through hydrophobic treatment, titanium dioxide, aluminium oxide, strontium titanates and
At least one of zinc stearate.
Realize that second object of the present invention can reach by adopting the following technical scheme that: a kind of ceramic carbon as described above
The preparation method of powder, includes the following steps:
Stock: prepare the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent；Dispersible pigment dispersion, wax
Mixed dispersion liquid with charge control agent is using surfactant as dispersion liquid；
Reaction: by the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent temperature be 40-55 DEG C
Under conditions of react, it is then cooling, filter, it is dry after external additive is added, obtain ceramic carbon dust.
Further, in dispersible pigment dispersion, the mass ratio of pigment and surfactant is 1:(0.05-0.5).
Further, in the mixed dispersion liquid of wax and charge control agent, the mixture of wax and charge control agent is living with surface
Property agent mass ratio be 1:(0.05-0.5).
Compared with prior art, the beneficial effects of the present invention are:
1, the ceramic carbon dust of the present invention has intact particle shape, relatively narrow particle diameter distribution and preferable mobility, can meet pottery
Porcelain carbon dust transferring rate is high, the high requirement of image density；
2, preparation method of the invention with the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent into
Row reaction, particle form larger micro particles in the liquid phase, the uniform carbon with appropriate particle size can be obtained under the conditions of temperature
Powder, it is uneven to avoid ceramic carbon dust electricity.
Specific embodiment
In the following, being described further in conjunction with specific embodiment to the present invention:
A kind of ceramics carbon dust, including following component by weight:
Wherein, resin includes acrylic resin and styrene resin with carboxyl functional group.
Acrylate with carboxyl functional group includes but is not limited to: methyl methacrylate, phenyl methacrylate, methyl
Ethyl acrylate, hydroxyethyl methacrylate, hydroxy propyl methacrylate, butyl methacrylate, methyl acrylate, acrylic acid
At least one of phenyl ester, ethyl acrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate and butyl acrylate.
Resin is used for carbon powder fixation, and the monomer with carboxyl functional group can provide more preferably paper wood adhesion, mainly mentions
For molecular weight appropriate, make resin liquid glue that there is certain characteristic, such as assembles fusion characteristics, paper wood adhesion and suitable glass and turn
Change temperature (Tg).
Wherein, pigment is based on black, yellow, carmetta and blue, and under normal circumstances, blue, black can select sharp crystalline substance
The inorganic pigment of stone class, such as cobalt blue spinelle, iron cobalt black spinelle, it is brilliant that nickel antimony titan yellow oxide, similar point can be selected in yellow
Zinc titan yellow of stone-type etc.；It is red etc. that chrome tin pink oxide, the cobalt powder of silicate-type can be selected in carmetta.
Wherein, charge control agent uses colourless, white or light-colored charge control agent, and including but not limited to negative electrical charge controls
Agent: at least one of chromium salicylate complex compound, zinc salicylate complex compound, salumin complex compound and salicylic acid zirconium complex；
It can also be positive charge control agent.
Wherein, the fusing point of wax is 65-155 DEG C, including but not limited to polypropylene wax, polyethylene wax, lignite wax, babassu
At least one of wax and synthetic wax.
Wherein, external additive is silica, titanium dioxide, aluminium oxide, strontium titanates and tristearin of the surface through hydrophobic treatment
At least one of sour zinc.
External additive is used to adjust the mobility and electrical property of ceramic carbon dust.
Resin in ceramic carbon dust can be prepared by polymerization reaction；The reaction temperature of polymerization reaction is 55-90 DEG C,
Mixing speed is 150-900rpm；Preferably, preparing the raw material that resin uses includes following component by weight:
Initiator includes but is not limited to ammonium persulfate or potassium peroxydisulfate；In addition, also may be used to effectively control molecular weight distribution
Chain-transferring agent, such as thio-alcohol is added.
The preparation method of ceramic carbon dust, includes the following steps:
Stock: prepare the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent；Dispersible pigment dispersion, wax
Mixed dispersion liquid with charge control agent is using surfactant as dispersion liquid；
Reaction: by the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent temperature be 40-55 DEG C
Under conditions of react, it is then cooling, filter, it is dry after external additive is added, obtain ceramic carbon dust.
Wherein, surfactant can be with are as follows:
Anionic surfactant includes but is not limited to: lauryl sodium sulfate, neopelex, dodecyl
Sodium naphthalene sulfonate, dialkylbenzene alkyl sulfate, dialkylbenzene alkylsulfonate and adipic acid etc.；
Cationic surfactant includes but is not limited to: alkyl phenyl alkyl dimethyl ammonium chloride, dialkyl phenyl organic dimethyl chloride
Change ammonium, alkyl phenyl ditallowdimethyl ammonium bromide etc.；
Surfactant can also be nonionic surfactant, such as polyoxyethylene cetyl ether, polyoxethylene octylphenyl
Phenyl ether, polyoxyethylene octyl ether, polyoxyethylene oleyl ether, Polyoxyethylene sorbitan monolaurate, polyoxyethylene
Stearyl ether, nonylphenol polyoxyethylene ether, dialkyl phenol polyoxyethylene ether etc..
In dispersible pigment dispersion, the mass ratio of pigment and surfactant is 1:(0.05-0.5)；
In the mixed dispersion liquid of wax and charge control agent, the mixture of wax and charge control agent, the matter with surfactant
The ratio between amount is 1:(0.05-0.5).
The dosage of surfactant adjusts the concentration of solution, and carbon dust partial size can be controlled in preparation method, reaches ingredient
Characteristic uniform, carried charge is uniform.
Preparation example 1:
Prepare resin emulsion:
210 parts of deionized waters and 2.5 parts of dodecyl sodium sulfates (anionic surfactant), are passed through nitrogen to reactor
To drain the air in reactor, heating makes the temperature of reaction system in reactor be maintained at 80 DEG C；Adjust stirring for agitating device
Mixing speed is about 250rpm；Then by 28 parts of butyl acrylates, 25 parts of Isobutyl methacrylates, 1 part of hydroxyethyl methacrylate second
Ester, 41 parts of styrene and 1.25 parts of lauryl mercaptans (chain-transferring agent) are slowly added in reactor, while 18.3g/L persulfuric acid is added dropwise
Potassium solution carries out polymerization reaction, time for adding 2h.
Gel permeation chromatograph GPC is used to measure the weight average molecular weight of polymer resin as 134000, number-average molecular weight is
12000, and when differential scan calorimeter DSC being used to measure glass transition temperature Tg as 59.5 DEG C, reaction system is cooled to room temperature,
It is filtered using 100 mesh filter screens, obtains cinepazid polymer emulsion, Gu containing the cinepazid polymer emulsion for 36.48%.
Preparation example 2:
Prepare the mixed dispersion liquid of wax and charge control agent:
By 50 parts of fusing points be about 81 DEG C Brazil wax and 50 parts of negative charge controlling agent DL-N24M (Hubei ancient cooking vessel dragon is holding
Limited liability company), 10 parts of neopelexes and 300 parts of deionized waters are stirred at 90 DEG C, and mixing speed is
Then pre-dispersed liquid is added to homogenous disperse in high pressure homogenizer by 800rpm, pre-dispersed 2h, using the American-European gram laser grain in Zhuhai
The particle size range that degree instrument LS900 measures dispersion liquid is 120-400nm, stops dispersion to get the mixing of wax and charge control agent is arrived
Dispersion liquid, solid content 24.39%.
Preparation example 3:
Prepare dispersible pigment dispersion:
15 parts of neopelexes are dissolved in 300 parts of deionized waters, 95 parts of 2900 (D50 of Black are added
0.52um) (BASF,F), after using 0.5h is dispersed with stirring under high speed shear dispersion machine 3000rpm speed, then will divide
Dispersion liquid strangles (PUHLER) grinder grinding distribution 1h with group, using measuring the particle size distribution range of dispersion liquid in 600-800nm
Stop grinding to get black pigment dispersion liquid, solid content 23.17% is arrived.
After 15 parts of neopelexes are dissolved in 300 parts of deionized waters, 95 parts of pigment blue Blue2502 (D50 are added
0.77um) (BASF,F), after being dispersed with stirring 0.5h under the speed of 3000rpm using high speed shear dispersion machine, then
(PUHLER) grinder grinding distribution 1h is strangled into dispersion liquid group, dispersion is measured using Zhuhai America and Europe gram laser particle analyzer LS900
The particle size distribution range of liquid stops grinding in 800-900nm to get Blue pigment dispersion liquid, solid content 23.17% is arrived.
After 15 parts of neopelexes are dissolved in 300 parts of deionized waters, 95 parts of Red Brown2700 (D50 are added
0.52um) (BASF,F), after being dispersed with stirring 0.5h under the speed of 3000rpm using high speed shear dispersion machine, then
(PUHLER) grinder grinding distribution 1h is strangled into dispersion liquid group, dispersion is measured using Zhuhai America and Europe gram laser particle analyzer LS900
The particle size distribution range of liquid stops grinding in 600-800nm to get Red Pigment Dispersion liquid, solid content 23.17% is arrived.
After 15 parts of neopelexes are dissolved in 300 parts of deionized waters, 95 parts of Yellow2200 (D50 are added
0.66um) (BASF,F), after being dispersed with stirring 0.5h under the speed of 3000rpm using high speed shear dispersion machine, then
(PUH LER) grinder grinding distribution 1h is strangled into dispersion liquid group, dispersion is measured using Zhuhai America and Europe gram laser particle analyzer LS900
The particle size distribution range of liquid stops grinding in 400-800nm to get Yellow Pigment Dispersion, solid content 23.17% is arrived.
Embodiment 1-5:
The ceramic carbon dust of embodiment 1-5, including constituent content as shown in Table 1:
The ceramic toner component parts by weight content of 1 embodiment 1-5 of table
| Ingredient | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Resin | 30 | 29 | 28 | 21 | 18 |
| Pigment | 60 | 65 | 70 | 75 | 80 |
| Charge control agent | 5 | 3 | 1 | 2 | 1 |
| Wax | 5 | 3 | 1 | 2 | 1 |
| External additive | 1 | 0.8 | 0.3 | 1 | 0.5 |
By the dispersible pigment dispersion and deionization in the mixed dispersion liquid of wax and charge control agent in preparation example 2, preparation example 3
Water is added in the reactor with agitating device, and adjusting mixing speed is 400rpm, and the benzene in preparation example 1 is added into reaction kettle
Third polymer emulsion with the pH value of pH meter detection mixture, is added dropwise with the speed of 15mL/min into reaction kettle after mixing evenly
The dilution heat of sulfuric acid that mass percent is 2%, makes the pH value 2.0 of the mixture in reaction kettle, then increases reaction system temperature
Degree keeps the temperature 5 hours to 45 DEG C, and using the grain diameter of the American-European gram of laser particle analyzer LS900 detection mixture in Zhuhai, works as partial size
When reaching about 12 μm, the sodium hydroxide solution that mass percent is 15% is added into reaction system, the pH of mixture is 7.5
When, stop heat preservation, and cool down to reaction system, be filtered, washed, dry, solid particulate matter is obtained, into solid particulate matter
It is added hydrophobic silica R812 (Evnoic Degussa (SEA) Pte., Ltd)；It is mixed, is obtained using Henschel mixer
Ceramic carbon dust.
Embodiment 1-5 is using the Red Pigment Dispersion liquid in preparation example 3.
Embodiment 6-8:
The ceramic carbon dust of embodiment 6-8, constituent content are as shown in Table 2:
The ceramic toner component parts by weight content of 2 embodiment 6-8 of table
| Ingredient | Embodiment 6 | Embodiment 7 | Embodiment 8 |
| Resin | 29 | 22 | 20 |
| Pigment | 67 | 70 | 74 |
| Charge control agent | 2 | 4 | 3 |
| Wax | 2 | 4 | 3 |
| External additive | 3 | 1 | 2 |
Embodiment 6 uses the Blue pigment dispersion liquid in preparation example 3；
Embodiment 7 uses the Yellow Pigment Dispersion in preparation example 3；
Embodiment 8 uses the black pigment dispersion liquid in preparation example 3.
The preparation method is the same as that of Example 1-5.
Detection:
The red ceramic carbon dust that embodiment 1-5 is obtained is printed upon water in Samsung laser printer ML1610 examination with computer
It on transfer paper, is then transferred on ceramic tile, is fired at 1200 DEG C.Print density on ceramic tile is tested, the results are shown in Table lattice 3.
The print density of 3 embodiment 1-5 of table
As can be seen from the table, embodiment 1-5 is in ceramic tile upper density 1.2 or more.From variable density it can be seen that face
Expect that the weight ratio in ceramic carbon dust can be 60-80%, preferably 65-75%.
The ceramic carbon dust that embodiment 4, embodiment 6,7,8 obtain is tested on Sharp color copy machine M X-3116N,
It is printed upon on water-transfer printing paper, is then transferred on ceramic tile, be fired at 1200 DEG C.Print density on ceramic tile is tested, is as a result seen
Table 4.
The print density of 4 embodiment 4 of table, 5-8
| Embodiment | Pigment percentage composition | Density |
| Embodiment 4 | 74.3% | 1.238 |
| Embodiment 6 | 65% | 1.257 |
| Embodiment 7 | 69.3% | 1.214 |
| Embodiment 8 | 72.5% | 1.336 |
Result above can be seen that ceramic carbon dust tests density height on Sharp color copy machine MX-3116N, and color is fresh
It is gorgeous.
For those skilled in the art, it can make other each according to the above description of the technical scheme and ideas
Kind is corresponding to be changed and deforms, and all these change and deform the protection model that all should belong to the claims in the present invention
Within enclosing.
Claims (10)
1. a kind of ceramics carbon dust, which is characterized in that including following component by weight:
2. ceramics carbon dust as described in claim 1, which is characterized in that including following component by weight:
3. ceramics carbon dust as described in claim 1, which is characterized in that the resin includes the acrylic acid tree with carboxyl functional group
Rouge and styrene resin.
4. ceramics carbon dust as described in claim 1, which is characterized in that the raw material for preparing the resin includes by weight
Following component:
5. ceramics carbon dust as described in claim 1, which is characterized in that the resin is prepared by polymerization reaction；It is described
The reaction temperature of polymerization reaction is 55-90 DEG C, mixing speed 150-900rpm.
6. ceramics carbon dust as described in claim 1, which is characterized in that the fusing point of the wax is 65-155 DEG C.
7. ceramics carbon dust as described in claim 1, which is characterized in that the external additive is dioxy of the surface through hydrophobic treatment
At least one of SiClx, titanium dioxide, aluminium oxide, strontium titanates and zinc stearate.
8. a kind of preparation method of ceramic carbon dust as described in claim 1, it is characterised in that include the following steps:
Stock: prepare the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent；The dispersible pigment dispersion, wax
Mixed dispersion liquid with charge control agent is using surfactant as dispersion liquid；
Reaction: the item for being 40-55 DEG C in temperature by the mixed dispersion liquid of resin emulsion, dispersible pigment dispersion, wax and charge control agent
It is reacted under part, external additive is added after then cooling, filtering, drying, obtains ceramic carbon dust.
9. the preparation method of ceramics carbon dust as claimed in claim 8, which is characterized in that in the dispersible pigment dispersion, pigment and table
The mass ratio of face activating agent is 1:(0.05-0.5).
10. the preparation method of ceramics carbon dust as claimed in claim 8, which is characterized in that the mixing of the wax and charge control agent
In dispersion liquid, the mixture of wax and charge control agent, the mass ratio with surfactant is 1:(0.05-0.5).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110426924A (en) * | 2019-07-12 | 2019-11-08 | 南京理工大学 | A kind of high pigment content ceramic inkpowder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6110632A (en) * | 1996-07-10 | 2000-08-29 | Cookson Matthey Ceramics Plc | Toner containing inorganic ceramic color |
| CN106033175A (en) * | 2015-03-17 | 2016-10-19 | 珠海艾派克微电子有限公司 | Color toner and preparation method thereof |
| CN106094455A (en) * | 2016-08-09 | 2016-11-09 | 广东丽格科技股份有限公司 | A kind of pottery carbon dust and preparation method thereof |
-
2018
- 2018-08-21 CN CN201810954167.XA patent/CN109240051A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6110632A (en) * | 1996-07-10 | 2000-08-29 | Cookson Matthey Ceramics Plc | Toner containing inorganic ceramic color |
| CN106033175A (en) * | 2015-03-17 | 2016-10-19 | 珠海艾派克微电子有限公司 | Color toner and preparation method thereof |
| CN106094455A (en) * | 2016-08-09 | 2016-11-09 | 广东丽格科技股份有限公司 | A kind of pottery carbon dust and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110426924A (en) * | 2019-07-12 | 2019-11-08 | 南京理工大学 | A kind of high pigment content ceramic inkpowder and preparation method thereof |
| CN110426924B (en) * | 2019-07-12 | 2023-08-22 | 南京理工大学 | Ceramic powdered ink with high pigment content and preparation method thereof |
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