CN106046859A - Black ceramic toner free of heavy metal and preparation method thereof - Google Patents
Black ceramic toner free of heavy metal and preparation method thereof Download PDFInfo
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- CN106046859A CN106046859A CN201610377233.2A CN201610377233A CN106046859A CN 106046859 A CN106046859 A CN 106046859A CN 201610377233 A CN201610377233 A CN 201610377233A CN 106046859 A CN106046859 A CN 106046859A
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- carbon black
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Classifications
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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
- C09C1/0009—Pigments for ceramics
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses black ceramic toner free of heavy metal and a preparation method thereof. The preparation method comprises the following steps of 1, preparation of a multi-walled carbon nanotube/carbon black compound; 2, preparation of multi-walled carbon nanotube/carbon black compound dispersion liquid; 3, preparation of ceramic black pigment. The multi-walled carbon nanotube/carbon black compound is adopted as a color generation body, the purpose of effectively lowering the cost is achieved, and the problem that the encapsulation rate is not high and the problem that the multi-walled carbon nanotube/carbon black compound is likely to be agglomerated in the preparation process are solved. The black ceramic toner has the advantages of being pure in color, easy to prepare, wide in raw material, low in price, easy to obtain and environmentally friendly, and can be applied to coloring ceramic glaze or blanks, and therefore the wide market space is achieved.
Description
Technical field
The present invention relates to technology of ceramic tile decoration field, particularly related to a kind of without heavy metal black ceramic toner
Preparation method.
Background technology
Along with the development of modern society, the use field of wall brick is also constantly being widened, the thing followed be wall brick not
This two big base attribute of the practicality of basic demand to be met, aesthetic property, beneficial environmental properties also becomes increasingly important.And do not contain
The wall brick of heavy metal, has exactly catered to modern and life staying idle at home has been pursued to the requirement of " green, environmental protection ".Make this product of wall brick
Product become " health escorts envoy " of people.
Instantly the black ceramic ink used on market is mainly by the heavy metallic oxide that can develop the color, silicate and aluminic acid
The ink that salt etc. are fired into colorant with other auxiliary materials and make.Using the heavy metal compound raw materials such as Zn, Pb, Cd, Sn
During making colorant, the pollution to environment, the injury to producers' health, all govern the development of ceramic ink, existing
Need a kind of method making nontoxic colorant without heavy metal raw material of research and development badly.
Summary of the invention
The technical problem to be solved there is provided a kind of preparation method without heavy metal black ceramic toner,
Overcome above-mentioned weak point.Present invention also offers a kind of without heavy metal black ceramic toner.
The technical problem to be solved is achieved by the following technical programs:
A kind of preparation method without heavy metal black ceramic toner, it comprises the steps:
(1) preparation of multi-walled carbon nano-tubes/carbon black complex: carbon black, multi-walled carbon nano-tubes are refluxed with concentrated nitric acid respectively 7 little
Time, with deionized water sucking filtration until neutrality, dry for standby, wherein, carbon black is 10:1 with the weight ratio of multi-walled carbon nano-tubes；By carboxylic
The carbon black of base and KH540 are under 72 DEG C of nitrogen protective conditions, and water-bath 3 hours, with deionized water sucking filtration until neutrality；In dilution
Ethanol solution in will the carbon black hydrolysis of grafting KH540, dried and functionalized multi-wall carbonnanotubes is in toluene, 62 DEG C of reactions
5 hours, after by product deionized water, dimethylbenzene sucking filtration until neutrality, remove unreacted carbon black, CNT, prepare bag
Coating particle multi-walled carbon nano-tubes/carbon black complex；
(2) preparation of multi-walled carbon nano-tubes/carbon black complex dispersion liquid: solvent by the 91.3% of weight percent content,
The dispersant of 0.7% pours pretreatment in high speed dispersion tank into, makes dispersant be dissolved completely in solvent；Add percentage by weight to contain
Multi-walled carbon nano-tubes/carbon black the complex of amount 8%, in described dispersant solvent, carries out disperseing to locate in advance with high-speed dispersion equipment
Reason, time 90min, dispersion frequency 40HZ, obtain multi-walled carbon nano-tubes/carbon black complex dispersion liquid A that solid content is 8%；
(3) according to tetraethyl orthosilicate: ethanol: the mass ratio=2.5:4:1 of water mixes, heating in water bath to 85 DEG C, with dilute nitre
Acid is catalyst, refluxes 8 hours and obtains Ludox；Then in Ludox, add aluminum nitrate, by mass percentage aluminum nitrate
For the 5.5% of Ludox, stirring and dissolving obtains solution B；Basic zirconium chloride is dissolved in ethanol: the volume ratio of water is the mixing of 1:1
In solvent, obtain saturated solution C；By dispersion liquid A, solution B, solution C mixing, the wherein mol ratio of Si:Zr in solution B, solution C
=1:(0.35 ~ 0.8), volume ratio=1:(125 ~ 135 of dispersion liquid A: solution B)；Heating mixed solution seethes with excitement to ethanol, then
Light ethanol and stop heating, after ethanol burns completely, i.e. obtaining the initial powder of black；Initial powder is ground to 250
Mesh, calcines 1 hour in temperature 800 ~ 1000 DEG C under argon shield, then cools down under argon shield, i.e. obtain ceramic black
Colorant.
In the present invention, the mol ratio=1:0.35 of Si:Zr, the volume of dispersion liquid A: solution B in described solution B, solution C
Ratio=1:135.
In the present invention, the mol ratio=1:0.5 of Si:Zr, the volume of dispersion liquid A: solution B in described solution B, solution C
Ratio=1:125.
In the present invention, the mol ratio=1:0.8 of Si:Zr, the volume of dispersion liquid A: solution B in described solution B, solution C
Ratio=1:130.
In the present invention, the mol ratio=1:0.5 of Si:Zr, the volume of dispersion liquid A: solution B in described solution B, solution C
Ratio=1:130.
A kind of by the above-mentioned preparation method without heavy metal black ceramic toner prepare without heavy metal black ceramic color
Powder.
There is advantages that the present invention is using multi-walled carbon nano-tubes/carbon black complex as in colour solid, it is achieved
Effectively reduce the purpose of cost, and solve the highest problem of encapsulation ratio and multi-walled carbon nano-tubes/carbon black complex in preparation process
In be easier to produce reunite problem；The black ceramic toner of the present invention has pure color, preparation is simple, raw material is extensive, valency
The honest and clean advantage being easy to get with environmental protection, can be applicable to the coloring in ceramic glaze or in base, therefore has wide market empty
Between.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It it not limitation of the invention.
Embodiment 1
A kind of without heavy metal black ceramic toner, it wraps up black pigment for Zirconium orthosilicate., and described black pigment is that many walls carbon is received
Mitron and carbon black complex.The preparation process of this black ceramic toner is as follows:
(1) preparation of multi-walled carbon nano-tubes/carbon black complex: carbon black, multi-walled carbon nano-tubes are refluxed with concentrated nitric acid respectively 7 little
Time, with deionized water sucking filtration until neutrality, dry for standby, wherein, carbon black is 10:1 with the weight ratio of multi-walled carbon nano-tubes；By carboxylic
The carbon black of base and KH540 are under 72 DEG C of nitrogen protective conditions, and water-bath 3 hours, with deionized water sucking filtration until neutrality；In dilution
Ethanol solution in will the carbon black hydrolysis of grafting KH540, dried and functionalized multi-wall carbonnanotubes is in toluene, 62 DEG C of reactions
5 hours, after by product deionized water, dimethylbenzene sucking filtration until neutrality, remove unreacted carbon black, CNT, prepare bag
Coating particle multi-walled carbon nano-tubes/carbon black complex；
(2) preparation of multi-walled carbon nano-tubes/carbon black complex dispersion liquid: solvent by the 91.3% of weight percent content,
The dispersant of 0.7% pours pretreatment in high speed dispersion tank into, makes dispersant be dissolved completely in solvent；Add percentage by weight to contain
Multi-walled carbon nano-tubes/carbon black the complex of amount 8%, in described dispersant solvent, carries out disperseing to locate in advance with high-speed dispersion equipment
Reason, time 90min, dispersion frequency 40HZ, obtain multi-walled carbon nano-tubes/carbon black complex dispersion liquid A that solid content is 8%；
(3) according to tetraethyl orthosilicate: ethanol: the mass ratio=2.5:4:1 of water mixes, heating in water bath to 85 DEG C, with dilute nitre
Acid is catalyst, refluxes 8 hours and obtains Ludox；Then in Ludox, add aluminum nitrate, by mass percentage aluminum nitrate
For the 5.5% of Ludox, stirring and dissolving obtains solution B；Basic zirconium chloride is dissolved in ethanol: the volume ratio of water is the mixing of 1:1
In solvent, obtain saturated solution C；By dispersion liquid A, solution B, solution C mixing, the wherein mol ratio of Si:Zr in solution B, solution C
=1:0.35, the volume ratio=1:135 of dispersion liquid A: solution B；Heating mixed solution seethes with excitement to ethanol, then lights ethanol and stops
Only heating, i.e. obtains the initial powder of black after ethanol burns completely；Initial powder is ground to 250 mesh, in argon shield
Under in temperature 800 ~ 1000 DEG C calcine 1 hour, then under argon shield cool down, i.e. obtain ceramic black colorant, its colorant in
Colour purity positive stabilization.
Embodiment 2
Based on embodiment 1, the difference is that only: the mol ratio=1:0.5 of Si:Zr, dispersion liquid A: solution in solution B, solution C
Volume ratio=the 1:125 of B；This colorant colour generation is pure stable.
Embodiment 3
Based on embodiment 1, the difference is that only: the mol ratio=1:0.8 of Si:Zr, dispersion liquid A: solution in solution B, solution C
Volume ratio=the 1:130 of B；This colorant colour generation is pure stable.
Embodiment 4
Based on embodiment 1, the difference is that only: the mol ratio=1:0.5 of Si:Zr, dispersion liquid A: solution in solution B, solution C
Volume ratio=the 1:130 of B；This colorant colour generation is pure stable.
Comparative example 1
Based on embodiment 1, the difference is that only: the volume ratio=1:100 of dispersion liquid A: solution B；This pure degree of colorant colour generation
Not.
Comparative example 2
Based on embodiment 1, the difference is that only: the volume ratio=1:200 of dispersion liquid A: solution B；This pure degree of colorant colour generation
Not.
Comparative example 3
Based on embodiment 1, the difference is that only: remove multi-walled carbon nano-tubes；This colorant colour generation poor instability of pure degree.
Embodiment 5
A kind of ceramic ink jet printing with without heavy metal black ink, containing the component of following mass percent: BYK161 4%,
Hydrocarbon organic solvent 20%, alcohol solvent 30%, NP-4 2%, Novalkyd 2550X70C 1%, black pigment 40%, polyether-modified
Siloxanes 0.5%, BYK051 0.4%, Disparlon NS-5501 0.1%；Described black pigment is the pottery obtained by embodiment 1
Porcelain black pigment.
The preparation method of ceramic ink jet printing black ink is as follows: component each in formula proportionally weighed, then
Carry out disperseing 40min with homogenizer；Scattered mixed liquor is loaded in grinder, grinds 10h, obtain particle diameter distribution≤
The ink semi-finished product of 1 μm；The agitator tank of semi-finished product ink is filled malleation, uses the strainer filtering of aperture≤1 μm, obtain finished product ink
Water.Wherein, the grinding bead of described grinder is the zirconium oxide bead of diameter 0.5 ~ 2nm, controls temperature of charge≤40 in process of lapping
℃。
Embodiment 6
A kind of ceramic ink jet printing with without heavy metal black ink, containing the component of following mass percent: BYK161 4%,
Hydrocarbon organic solvent 25%, alcohol solvent 30%, NP-4 2%, Novalkyd 2550X70C 1%, black pigment 35%, polyether-modified
Siloxanes 0.5%, BYK051 0.4%, Disparlon NS-5501 0.1%；Described black pigment is the pottery obtained by embodiment 2
Porcelain black pigment.
The preparation method of ceramic ink jet printing black ink is as follows: component each in formula proportionally weighed, then
Carry out disperseing 40min with homogenizer；Scattered mixed liquor is loaded in grinder, grinds 10h, obtain particle diameter distribution≤
The ink semi-finished product of 1 μm；The agitator tank of semi-finished product ink is filled malleation, uses the strainer filtering of aperture≤1 μm, obtain finished product ink
Water.Wherein, the grinding bead of described grinder is the zirconium oxide bead of diameter 0.5 ~ 2nm, controls temperature of charge≤40 in process of lapping
℃。
Embodiment 7
A kind of ceramic ink jet printing with without heavy metal black ink, containing the component of following mass percent: BYK161 4%,
Hydrocarbon organic solvent 25%, alcohol solvent 35%, NP-4 2%, Novalkyd 2550X70C 1%, black pigment 30%, polyether-modified
Siloxanes 0.5%, BYK051 0.4%, Disparlon NS-5501 0.1%；Described black pigment is the pottery obtained by embodiment 3
Porcelain black pigment.
The preparation method of ceramic ink jet printing black ink is as follows: component each in formula proportionally weighed, then
Carry out disperseing 40min with homogenizer；Scattered mixed liquor is loaded in grinder, grinds 10h, obtain particle diameter distribution≤
The ink semi-finished product of 1 μm；The agitator tank of semi-finished product ink is filled malleation, uses the strainer filtering of aperture≤1 μm, obtain finished product ink
Water.Wherein, the grinding bead of described grinder is the zirconium oxide bead of diameter 0.5 ~ 2nm, controls temperature of charge≤40 in process of lapping
℃。
Embodiment 8
A kind of ceramic ink jet printing with without heavy metal black ink, containing the component of following mass percent: BYK161 4%,
Hydrocarbon organic solvent 23%, alcohol solvent 35%, NP-4 2%, Novalkyd 2550X70C 1%, black pigment 32%, polyether-modified
Siloxanes 0.5%, BYK051 0.4%, Disparlon NS-5501 0.1%；Described black pigment is the pottery obtained by embodiment 1
Porcelain black pigment.
The preparation method of ceramic ink jet printing black ink is as follows: component each in formula proportionally weighed, then
Carry out disperseing 40min with homogenizer；Scattered mixed liquor is loaded in grinder, grinds 10h, obtain particle diameter distribution≤
The ink semi-finished product of 1 μm；The agitator tank of semi-finished product ink is filled malleation, uses the strainer filtering of aperture≤1 μm, obtain finished product ink
Water.Wherein, the grinding bead of described grinder is the zirconium oxide bead of diameter 0.5 ~ 2nm, controls temperature of charge≤40 in process of lapping
℃。
Ceramic ink jet printing black ink prepared by embodiment 5 ~ 8 is carried out performance test, and test result see table.By
Table understands, and the black ink of the ceramic ink jet printing prepared by the present invention has good stability and Ink Jet Printing Performance.
Embodiment described above only have expressed embodiments of the present invention, and it describes more concrete and detailed, but can not
Therefore the restriction to the scope of the claims of the present invention it is interpreted as, as long as using the skill that the form of equivalent or equivalent transformation is obtained
Art scheme, all should fall within the scope and spirit of the invention.
Claims (6)
1. the preparation method without heavy metal black ceramic toner, it comprises the steps:
(1) preparation of multi-walled carbon nano-tubes/carbon black complex: carbon black, multi-walled carbon nano-tubes are refluxed with concentrated nitric acid respectively 7 little
Time, with deionized water sucking filtration until neutrality, dry for standby, wherein, carbon black is 10:1 with the weight ratio of multi-walled carbon nano-tubes；By carboxylic
The carbon black of base and KH540 are under 72 DEG C of nitrogen protective conditions, and water-bath 3 hours, with deionized water sucking filtration until neutrality；In dilution
Ethanol solution in will the carbon black hydrolysis of grafting KH540, dried and functionalized multi-wall carbonnanotubes is in toluene, 62 DEG C of reactions
5 hours, after by product deionized water, dimethylbenzene sucking filtration until neutrality, remove unreacted carbon black, CNT, prepare bag
Coating particle multi-walled carbon nano-tubes/carbon black complex；
(2) preparation of multi-walled carbon nano-tubes/carbon black complex dispersion liquid: solvent by the 91.3% of weight percent content,
The dispersant of 0.7% pours pretreatment in high speed dispersion tank into, makes dispersant be dissolved completely in solvent；Add percentage by weight to contain
Multi-walled carbon nano-tubes/carbon black the complex of amount 8%, in described dispersant solvent, carries out disperseing to locate in advance with high-speed dispersion equipment
Reason, time 90min, dispersion frequency 40HZ, obtain multi-walled carbon nano-tubes/carbon black complex dispersion liquid A that solid content is 8%；
(3) according to tetraethyl orthosilicate: ethanol: the mass ratio=2.5:4:1 of water mixes, heating in water bath to 85 DEG C, with dilute nitre
Acid is catalyst, refluxes 8 hours and obtains Ludox；Then in Ludox, add aluminum nitrate, by mass percentage aluminum nitrate
For the 5.5% of Ludox, stirring and dissolving obtains solution B；Basic zirconium chloride is dissolved in ethanol: the volume ratio of water is the mixing of 1:1
In solvent, obtain saturated solution C；By dispersion liquid A, solution B, solution C mixing, the wherein mol ratio of Si:Zr in solution B, solution C
=1:(0.35 ~ 0.8), volume ratio=1:(125 ~ 135 of dispersion liquid A: solution B)；Heating mixed solution seethes with excitement to ethanol, then
Light ethanol and stop heating, after ethanol burns completely, i.e. obtaining the initial powder of black；Initial powder is ground to 250
Mesh, calcines 1 hour in temperature 800 ~ 1000 DEG C under argon shield, then cools down under argon shield, i.e. obtain ceramic black
Colorant.
Preparation method without heavy metal black ceramic toner the most according to claim 1, it is characterised in that described solution
Mol ratio=the 1:0.35 of Si:Zr in B, solution C, the volume ratio=1:135 of dispersion liquid A: solution B.
Preparation method without heavy metal black ceramic toner the most according to claim 1, it is characterised in that described solution
Mol ratio=the 1:0.5 of Si:Zr in B, solution C, the volume ratio=1:125 of dispersion liquid A: solution B.
Preparation method without heavy metal black ceramic toner the most according to claim 1, it is characterised in that described solution
Mol ratio=the 1:0.8 of Si:Zr in B, solution C, the volume ratio=1:130 of dispersion liquid A: solution B.
Preparation method without heavy metal black ceramic toner the most according to claim 1, it is characterised in that described solution
Mol ratio=the 1:0.5 of Si:Zr in B, solution C, the volume ratio=1:130 of dispersion liquid A: solution B.
6. what prepared by the preparation method without heavy metal black ceramic toner as described in claim 1 is black without heavy metal
Color pottery toner.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610377233.2A CN106046859A (en) | 2016-06-01 | 2016-06-01 | Black ceramic toner free of heavy metal and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610377233.2A CN106046859A (en) | 2016-06-01 | 2016-06-01 | Black ceramic toner free of heavy metal and preparation method thereof |
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| CN106046859A true CN106046859A (en) | 2016-10-26 |
Family
ID=57172358
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| CN1791474A (en) * | 2003-05-16 | 2006-06-21 | 布卢薄膜有限责任公司 | Method for coating substrates with a carbon-based material |
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