CN112592608A - Oil-soluble dye coupled nano carbon black and preparation method thereof - Google Patents
Oil-soluble dye coupled nano carbon black and preparation method thereof Download PDFInfo
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- CN112592608A CN112592608A CN202011289945.1A CN202011289945A CN112592608A CN 112592608 A CN112592608 A CN 112592608A CN 202011289945 A CN202011289945 A CN 202011289945A CN 112592608 A CN112592608 A CN 112592608A
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- carbon black
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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
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
- C09D11/326—Inkjet printing inks characterised by colouring agents containing carbon black characterised by the pigment dispersant
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a technical method for improving the covering power and hue plumpness of nano carbon black by adding oil-soluble blue dye, and simultaneously, the blue dye can be effectively prevented from migrating through a coupling process, the phenomenon that the system is bluish due to migration and surface enrichment of the blue dye during later use of the nano carbon black is prevented, the storage stability of the nano carbon black is improved, agglomeration is effectively prevented, and the dispersion performance of the nano carbon black is enhanced.
Description
Technical Field
The invention relates to the technical field of nano carbon black modification, in particular to oil-soluble dye coupled nano carbon black and a preparation method thereof.
Background
The nano carbon black has excellent colorability, weather resistance and chemical stability, is rich in source and low in price, is one of important coloring agents, but has poor stability and poor surface color effect although strong hiding power due to the characteristics of small particle size, large specific surface area, easiness in agglomeration and the like of nano carbon black particles and the fact that the color effect presented in an ink system is dull, dull and lusterless.
In the practical application of the nano carbon black, a blue dye is generally added into an ink system at the same time to improve the covering power and the glossiness of the ink and simultaneously appear darker. However, such an operation has a problem that: since the blue dye is soluble in the ink system, the blue dye is prone to blue after the ink is cured and to deviate from a pure black color due to the phenomena of dye migration and surface enrichment after the ink is stored, sprayed or coated.
Meanwhile, the nano carbon black has a large specific surface area, and is easy to agglomerate during storage, so that the particle volume is increased, the nano carbon black can be dispersed only by long-time high-strength shearing or sanding during actual use, the production efficiency is low, and the energy consumption is high.
Disclosure of Invention
The invention provides oil-soluble dye coupled nano carbon black and a preparation method thereof, which can effectively prevent blue dye from migrating through a coupling process while improving the covering power and the glossiness of the nano carbon black, prevent the blue dye from migrating and surface enrichment to cause the bluing phenomenon of a system during later use of the nano carbon black, improve the storage stability of the nano carbon black, effectively prevent agglomeration and enhance the dispersion performance of the nano carbon black.
An oil-soluble dye coupled nano carbon black, which is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 3-5 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.2-0.8 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epoxy chloropropane accounting for 1-5% of the mass of the nano carbon black, uniformly dispersing, heating to 55-65 ℃, and reacting for 1-2 h;
(4) continuously adding liquid paraffin accounting for 2-4% of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
Further, the particle size of the nano carbon black is 20nm-60 nm.
Further, the oil-soluble blue dye in step (2) may be one or more of solvent blue 36, solvent blue 45 and solvent blue 63.
Further, the liquid paraffin has a boiling point higher than 270 ℃.
Further, the reduced pressure spray drying process in the step (4) is carried out at a vacuum degree of-0.07 MPa to-0.09 MPa and a temperature of 75-80 ℃.
The oil-soluble dye coupled nano carbon black can be used for ink-jet ink, silk-screen ink, flexo ink and offset ink, and is particularly suitable for an oily system.
The invention has the technical effects and advantages that:
1. according to the invention, the covering power and the glossiness of the nano carbon black are effectively improved by adding the blue dye;
2. according to the invention, through a coupling process, blue dye migration can be effectively prevented, and the phenomenon that the blue dye migrates and the surface is enriched to cause system bluing in the later use of the nano carbon black is prevented;
3. according to the invention, the liquid paraffin is added as the dispersion stabilizer, so that the storage stability of the dispersion stabilizer is greatly improved, the agglomeration can be effectively prevented, the dispersion performance is enhanced, the production efficiency is improved during use, and the energy consumption can be reduced.
Detailed Description
Example 1
An oil-soluble dye coupled nano carbon black, which is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 3 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.2 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epoxy chloropropane accounting for 1 percent of the mass of the nano carbon black, uniformly dispersing, heating to 55 ℃, and reacting for 1 hour;
(4) continuously adding liquid paraffin accounting for 2 percent of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The oil-soluble blue dye in the step (2) is solvent blue 36.
The liquid paraffin has a boiling point above 270 ℃.
The reduced pressure spray drying process in the step (4) is carried out at the vacuum degree of-0.07 MPa and the temperature of 80 ℃.
Example 2
An oil-soluble dye coupled nano carbon black, which is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 4 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.5 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epoxy chloropropane accounting for 3 percent of the mass of the nano carbon black, uniformly dispersing, heating to 60 ℃, and reacting for 1.5 hours;
(4) continuously adding liquid paraffin accounting for 3% of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The oil-soluble blue dye in the step (2) is solvent blue 45.
The liquid paraffin has a boiling point above 270 ℃.
The reduced pressure spray drying process in the step (4) is carried out at the vacuum degree of-0.08 MPa and the temperature of 78 ℃.
Example 3
An oil-soluble dye coupled nano carbon black, which is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 5 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.8 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epichlorohydrin with the mass of 5% of the nano carbon black, uniformly dispersing, heating to 65 ℃, and reacting for 2 hours;
(4) continuously adding liquid paraffin accounting for 4% of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The oil-soluble blue dye in the step (2) is solvent blue 63.
The liquid paraffin has a boiling point above 270 ℃.
The reduced pressure spray drying process in the step (4) is carried out at the vacuum degree of-0.09 MPa and the temperature of 75 ℃.
Example 4
The same procedure as in example 2 was repeated except that no liquid paraffin was added in the step (4).
Example 5
An oil-soluble dye coupled nano carbon black, which is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 2 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.1 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epoxy chloropropane with the mass of 5.5 percent of the nano carbon black, uniformly dispersing, heating to 68 ℃, and reacting for 2.5 h;
(4) continuously adding liquid paraffin accounting for 1.5 percent of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The oil-soluble blue dye in the step (2) is solvent blue 45.
The boiling point of the liquid paraffin is 250 ℃.
The reduced pressure spray drying process in the step (4) is carried out at the vacuum degree of-0.06 MPa and the temperature of 70 ℃.
Comparative example 1
The nano carbon black feedstock of example 2 was taken without treatment by the process of the present invention.
Comparative example 2
A nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 4 times, and uniformly stirring;
(2) then adding oil-soluble blue dye with the mass of 0.5 per mill of the nano carbon black, and uniformly dispersing;
(3) after the dispersion is uniform, reduced pressure spray drying is carried out;
(4) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The oil-soluble blue dye in the step (2) is solvent blue 45.
The reduced pressure spray drying process in the step (3) is carried out at the vacuum degree of-0.08 MPa and the temperature of 78 ℃.
Comparative example 3
A nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 4 times, and uniformly stirring;
(2) adding liquid paraffin accounting for 3% of the mass of the nano carbon black, uniformly dispersing, and then carrying out reduced pressure spray drying;
(3) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The liquid paraffin has a boiling point above 270 ℃.
The reduced pressure spray drying process in the step (2) is carried out at the vacuum degree of-0.08 MPa and the temperature of 78 ℃.
Comparative example 4
A nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 4 times, and uniformly stirring;
(2) adding liquid paraffin accounting for 3% of the mass of the nano carbon black, uniformly dispersing, and then carrying out reduced pressure spray drying;
(3) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The boiling point of the liquid paraffin is 250 ℃.
The reduced pressure spray drying process in the step (2) is carried out at the vacuum degree of-0.08 MPa and the temperature of 78 ℃.
And (3) effect comparison:
1. hiding power and gloss: taking oil gloss oil, adding the nano carbon black prepared in each example and each comparative example in a mass ratio of 1:10 without adding a wetting dispersant, and grinding for 2 hours by a sand mill to obtain sample ink; spraying and curing, observing whether a bluing phenomenon exists or not in a backlight manner, and testing the blackness, the covering power and the glossiness of each sample; meanwhile, the sample ink is subjected to a particle size test (D50), and a storage experiment is carried out, wherein the storage interval is 7 days;
the testing method of the blackness is to measure the L value by an image spectrum colorimeter in a 10-degree view angle according to an SCE mode;
the testing method of the covering power is GB/T1726-1979 coating covering power determination method: the covering power X of the spray coating method is (W2-W1) × 100, and the unit is g/m2；
W2 is the quality of the glass plate after spraying, and W1 is the quality of the glass plate before spraying;
the glossiness is measured by a 60-degree ink glossiness instrument, the glossiness of the ink is expressed by the specular glossiness, and the unit is that the higher the percentage of the glossiness is, the better the surface specular effect is;
2. degree of pigment liberation: testing an absorbance curve (a solvent system is petroleum ether) of the oil-soluble blue dye, adding the nano carbon black prepared in each embodiment and the comparative example in a mass ratio of 1:99 of the nano carbon black to the petroleum ether, uniformly stirring, centrifuging, taking supernatant liquid to measure absorbance to obtain free pigment, and dividing the free pigment by the total pigment to obtain the free pigment ratio;
3. storage stability: the nano carbon black prepared in each example and the comparative example is subjected to a storage experiment, and after the nano carbon black is stored for 1 month, 2 months and 3 months, the agglomeration condition of the nano carbon black is tested by using a laser particle size analyzer, wherein the method is a dry method for directly measuring the particle size of the nano carbon black agglomerate.
TABLE 1
As can be seen from Table 1, the blackness and the covering power of the oil-soluble dye-coupled nano carbon black prepared by the method are obviously improved, the mirror surface gloss is also obviously improved, and after the liquid paraffin is added, the oil-soluble dye-coupled nano carbon black has good dispersibility, is not easy to agglomerate, and has obviously improved stability.
TABLE 2
As can be seen from Table 2, the oil-soluble dye-coupled nano carbon black prepared by the method has a good coupling effect on the dye, is not easy to dissolve out, and can effectively reduce the phenomenon of surface enrichment and bluing caused by dissociation in the later use process. Meanwhile, after the coupling process and the addition of the liquid paraffin, the storage stability of the nano carbon black is remarkably improved, so that the grinding and dispersion in later use are greatly facilitated, the production efficiency can be effectively improved, and the energy consumption can be reduced.
The above examples and comparative examples select the nano carbon black with the particle size of 40nm for experimental comparison, and the process of the present invention is also effective for the nano carbon black with the particle sizes of 20nm and 60nm, and the experimental results thereof basically follow the same rules as the above experiments.
The above examples and comparative examples are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention has been described in detail by the above examples and comparative examples, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the present invention as defined by the claims.
Claims (7)
1. An oil-soluble dye coupled nano carbon black is characterized in that: the preparation method of the nano carbon black comprises the following steps:
(1) dispersing the nano carbon black in petroleum ether with the mass multiple of 3-5 times, and uniformly stirring;
(2) adding oil-soluble blue dye with the mass of 0.2-0.8 per mill of the nano carbon black, and uniformly dispersing;
(3) then adding epoxy chloropropane accounting for 1-5% of the mass of the nano carbon black, uniformly dispersing, heating to 55-65 ℃, and reacting for 1-2 h;
(4) continuously adding liquid paraffin accounting for 2-4% of the mass of the nano carbon black after the reaction is finished, uniformly dispersing, performing reduced pressure spray drying, and recovering petroleum ether to the step (1) to obtain the oil-soluble dye coupled nano carbon black;
(5) sealing, packaging, and storing in waterproof mode for later use.
2. The oil-soluble dye-coupled carbon black according to claim 1, wherein: the particle size of the nano carbon black is 20nm-60 nm.
3. The oil-soluble dye-coupled carbon black according to claim 1, wherein: the oil-soluble blue dye in the step (2) can be one or more of solvent blue 36, solvent blue 45 and solvent blue 63.
4. The oil-soluble dye-coupled carbon black according to claim 1, wherein: the liquid paraffin has a boiling point above 270 ℃.
5. The oil-soluble dye-coupled carbon black according to claim 1, wherein: the reduced pressure spray drying process in the step (4) has the vacuum degree of minus 0.07MPa to minus 0.09MPa and the temperature of 75 ℃ to 80 ℃.
6. The oil-soluble dye-coupled carbon black according to any one of claims 1 to 5, wherein: the oil-soluble dye coupled nano carbon black can be used for ink-jet ink, silk-screen ink, flexo ink and offset ink.
7. The oil-soluble dye-coupled carbon black according to any one of claims 1 to 5, wherein: the oil-soluble dye coupled nano carbon black can be used for oil paint or oil printing ink.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539819A (en) * | 2022-01-20 | 2022-05-27 | 中昊黑元化工研究设计院有限公司 | Preparation method of oil-soluble nano carbon black slurry |
Citations (3)
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|---|---|---|---|---|
| US3963510A (en) * | 1973-11-08 | 1976-06-15 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of toned carbon black |
| CN106566290A (en) * | 2016-11-11 | 2017-04-19 | 青岛科技大学 | White carbon black with dyeing groups on surface and preparation method of white carbon black |
| CN109054462A (en) * | 2018-06-22 | 2018-12-21 | 确成硅化学股份有限公司 | A method of it improving white carbon black and prevents old performance |
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2020
- 2020-11-17 CN CN202011289945.1A patent/CN112592608B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3963510A (en) * | 1973-11-08 | 1976-06-15 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of toned carbon black |
| CN106566290A (en) * | 2016-11-11 | 2017-04-19 | 青岛科技大学 | White carbon black with dyeing groups on surface and preparation method of white carbon black |
| CN109054462A (en) * | 2018-06-22 | 2018-12-21 | 确成硅化学股份有限公司 | A method of it improving white carbon black and prevents old performance |
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| Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539819A (en) * | 2022-01-20 | 2022-05-27 | 中昊黑元化工研究设计院有限公司 | Preparation method of oil-soluble nano carbon black slurry |
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