CN112358749B - Water-soluble dye coupled nano carbon black and preparation method thereof - Google Patents
Water-soluble dye coupled nano carbon black and preparation method thereof Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer 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
- C09C3/10—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
- 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
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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
- 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
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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
- 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
- C09D11/328—Inkjet printing inks characterised by colouring agents characterised by dyes
Abstract
The invention discloses a technical method for improving the covering power and hue plumpness of nano carbon black by adding water-soluble blue dye, and simultaneously, the blue dye can be effectively prevented from migrating through a coupling process, the phenomenon that the blue dye migrates and the surface is enriched to cause the bluing of a system when the nano carbon black is used in the later period is prevented, the storage stability of the nano carbon black is improved, the 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 water-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 colorants, but 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 and most of the nano carbon black particles show a red phase, the defects cause poor stability of the nano carbon black ink, and the nano carbon black ink has strong hiding power but has poor surface color effect.
In the practical application of nano carbon black, a blue dye is generally added into an ink system at the same time to improve the hiding power of the ink and adjust the color phase, and the black ink with the blue color phase is 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 stored, sprayed or coated, and phenomena of dye migration and surface enrichment occur, so that the ink is prone to blue after being cured, and printed matters have color deviation.
Meanwhile, the nano carbon black has a large specific surface area, is easy to agglomerate during storage, causes the particle volume to increase, and can be dispersed only by long-time high-strength shearing or sanding during actual use in ink, so that the production efficiency is low, and the energy consumption is high.
Disclosure of Invention
The invention provides water-soluble dye coupling type nano carbon black and a preparation method thereof, which can effectively prevent blue dye from migrating, prevent the blue dye from migrating and surface enrichment from causing the bluing phenomenon of a system when the nano carbon black is used in a later period, improve the storage stability of the nano carbon black, effectively prevent agglomeration and enhance the dispersion performance of the nano carbon black while improving the covering power and the glossiness of the nano carbon black and adjusting the hue.
A water-soluble dye coupling type nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 3-5 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 1-5% of the nano carbon black, uniformly dispersing, heating to 40-50 ℃, and stirring for 30-50 min;
(3) then adding water-soluble blue dye with the mass of 0.2-0.8 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent accounting for 1-3% of the mass of the nano carbon black, adjusting the temperature to 45-55 ℃, and reacting for 1-2 hours;
(5) after the reaction is finished, continuously adding Arabic gum accounting for 1-2% of the mass of the nano carbon black, uniformly dispersing, and performing reduced pressure spray drying to obtain the water-soluble dye coupled nano carbon black;
(6) sealing, packaging, and storing in waterproof mode for later use.
Furthermore, the particle size of the nano carbon black is 20nm-60 nm.
Further, the water-soluble blue dye in step (3) may be one or more of GT-820, direct blue 2B, and direct blue 15.
Further, the silane coupling agent in step (4) may be one or more of KH550, KH560 and KH 570.
Further, the reduced pressure spray drying process in the step (5) has the vacuum degree of-0.07 MPa to-0.09 MPa and the temperature of 55 ℃ to 60 ℃.
The water-soluble dye coupled nano carbon black can be used for ink-jet ink, screen printing ink, flexible printing ink and offset printing ink, and is particularly suitable for a water-based system.
The invention has the technical effects and advantages that:
1. according to the invention, the blue dye is added to the surface of the nano carbon black in advance, so that the hue of the ink can be adjusted, and the covering power and the glossiness of the nano carbon black are effectively improved;
2. according to the invention, the blue dye is coated on the surface of the nano carbon black through a coupling process, so that the blue dye can be effectively prevented from migrating, and the phenomenon that the blue dye is easy to migrate and surface enriched to cause system bluing when the blue dye is used in ink at a later stage is prevented;
3. according to the invention, the Arabic gum is added as a dispersion stabilizer, so that the storage stability of the Arabic gum 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
A water-soluble dye coupling type nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 3 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 1% of that of the nano carbon black, uniformly dispersing, heating to 40 ℃, and stirring for 50 min;
(3) then adding water-soluble blue dye with the mass of 0.2 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent accounting for 1 percent of the mass of the nano carbon black, adjusting the temperature to 55 ℃, and reacting for 1 hour;
(5) after the reaction is finished, continuously adding Arabic gum accounting for 1 percent of the mass of the nano carbon black, uniformly dispersing, and performing reduced pressure spray drying to obtain the water-soluble dye coupled nano carbon black;
(6) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The water-soluble blue dye in step (3) is GT-820.
The silane coupling agent in the step (4) is KH 550.
The reduced pressure spray drying process in the step (5) is carried out at the vacuum degree of-0.09 MPa and the temperature of 55 ℃.
Example 2
A water-soluble dye coupling type nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 4 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 3% of that of the nano carbon black, uniformly dispersing, heating to 45 ℃, and stirring for 40 min;
(3) then adding water-soluble blue dye with the mass of 0.5 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent accounting for 2 percent of the mass of the nano carbon black, adjusting the temperature to 50 ℃, and reacting for 1.5 hours;
(5) after the reaction is finished, continuously adding Arabic gum accounting for 1.5 percent of the mass of the nano carbon black, uniformly dispersing, and performing reduced pressure spray drying to obtain the water-soluble dye coupled nano carbon black;
(6) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The water-soluble blue dye in the step (3) is direct blue 2B.
The silane coupling agent in the step (4) is KH 560.
The reduced pressure spray drying process in the step (5) is carried out at vacuum degree of-0.08 MPa and temperature of 58 ℃.
Example 3
A water-soluble dye coupling type nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 5 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 5% of that of the nano carbon black, uniformly dispersing, heating to 50 ℃, and stirring for 30 min;
(3) then adding water-soluble blue dye with the mass of 0.8 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent accounting for 3% of the mass of the nano carbon black, adjusting the temperature to 45 ℃, and reacting for 2 hours;
(5) after the reaction is finished, continuously adding Arabic gum accounting for 2% of the mass of the nano carbon black, uniformly dispersing, and performing reduced pressure spray drying to obtain the water-soluble dye coupled nano carbon black;
(6) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The water-soluble blue dye in the step (3) is direct blue 15.
The silane coupling agent in the step (4) is KH 570.
The reduced pressure spray drying process in the step (5) is carried out at the vacuum degree of-0.07 MPa and the temperature of 60 ℃.
Example 4
Step (5) was performed without adding gum arabic, as in example 2.
Example 5
A water-soluble dye coupling type nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 2 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 0.8 percent of that of the nano carbon black, uniformly dispersing, heating to 55 ℃, and stirring for 60 min;
(3) then adding water-soluble blue dye with the mass of 0.1 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent accounting for 4% of the mass of the nano carbon black, adjusting the temperature to 60 ℃, and reacting for 2.5 hours;
(5) after the reaction is finished, continuously adding Arabic gum with the mass of 0.8% of that of the nano carbon black, uniformly dispersing, and performing reduced pressure spray drying to obtain the water-soluble dye coupling type nano carbon black;
(6) sealing, packaging, and storing in waterproof mode for later use.
The particle size of the nano carbon black is 40 nm.
The water-soluble blue dye in the step (3) is direct blue 2B.
The silane coupling agent in the step (4) is KH 560.
The reduced pressure spray drying process in the step (5) is carried out at the vacuum degree of-0.06 MPa and the temperature of 65 ℃.
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 pure water with the mass multiple of 4 times, and uniformly stirring;
(2) then adding water-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 water-soluble blue dye in the step (2) is direct blue 2B.
The reduced pressure spray drying process in the step (3) is carried out at vacuum degree of-0.08 MPa and temperature of 58 ℃.
Comparative example 3
A nano carbon black is prepared by the following steps:
(1) dispersing the nano carbon black in pure water with the mass multiple of 4 times, and uniformly stirring;
(2) adding Arabic gum accounting for 1.5 percent 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 reduced pressure spray drying process in the step (2) is carried out at vacuum degree of-0.08 MPa and temperature of 58 ℃.
And (3) effect comparison:
1. hiding power and gloss: taking water-based varnish, adding the nano carbon black prepared in each example and the 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: spray coating method
Hiding power X ═ 100 (W2-W1) in 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 of the water-soluble blue dye, adding the nano carbon black prepared in each embodiment and the comparative example according to the mass ratio of the nano carbon black to the water of 1:99, uniformly stirring, centrifuging, taking the supernatant to measure the absorbance to obtain the 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 water-soluble dye-coupled nano carbon black prepared by the method has the advantages of obviously improved blackness and hiding power, obviously improved mirror surface gloss, good dispersing performance, difficult agglomeration and obviously improved stability after the Arabic gum is added.
TABLE 2
As can be seen from Table 2, the water-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 Arabic gum, 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 (3)
1. A water-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 pure water with the mass multiple of 4 times, and uniformly stirring;
(2) adding hydrogen peroxide with the mass of 3% of that of the nano carbon black, uniformly dispersing, heating to 45 ℃, and stirring for 40 min;
(3) then adding water-soluble blue dye direct blue 2B with the mass of 0.5 per mill of the nano carbon black, and uniformly dispersing;
(4) adding a silane coupling agent KH560 accounting for 2% of the mass of the nano carbon black, adjusting the temperature to 50 ℃, and reacting for 1.5 h;
(5) after the reaction is finished, continuously adding Arabic gum with the mass of 1.5 percent of that of the nano carbon black, uniformly dispersing, and then carrying out reduced pressure spray drying, wherein the reduced pressure spray drying process is that the vacuum degree is-0.08 MPa, and the temperature is 58 ℃, so as to obtain the water-soluble dye coupling type nano carbon black;
(6) sealing and packaging, and storing in a waterproof way for later use;
the particle size of the nano carbon black is 40 nm.
2. The water-soluble dye-coupled carbon black according to claim 1, wherein: the water-soluble dye coupled nano carbon black is used for ink-jet ink, silk-screen ink, flexible printing ink and offset printing ink.
3. The water-soluble dye-coupled carbon black according to claim 1, wherein: the water-soluble dye coupled nano carbon black is used for water-based paint or water-based ink.
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