96801-39-7 Purity
98%+
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Specification
Styrene-maleic acid copolymers were synthesized by free radical polymerization. Encapsulated pigment red 122 dispersions were prepared by sedimentation using these copolymers. The effects of copolymer structure such as the molar content of maleic acid, molecular weight and amount of copolymer on the stability and particle size of the dispersion were studied. The results showed that the encapsulated pigment dispersion had higher stability and smaller particle size. When the molar content of maleic acid was 0.43, the intrinsic viscosity was 79.65 ml/g and the amount of copolymer was 10%, a narrow particle distribution could be obtained. The thickness of the encapsulation layer was observed to be about 5nm by TEM.
A certain amount of PSMA was dissolved in a solvent, and then a corresponding amount of pigment red 122 filter cake was added to the solution under stirring. The mixed slurry was transferred to disperse at 4000 rpm for 1 h, and an adsorption promoter that could reduce the solubility of PSMA in the solvent was added to the slurry, and PSMA was slowly deposited and encapsulated on the surface of the pigment. The mixture was vacuum filtered and dried in an oven at 45°C for 24 hours to obtain the encapsulated pigment. Prepare a dispersion with 5 grams of encapsulated pigment and 95 grams of distilled water, adjust the pH to 8 with sodium hydroxide solution, heat and stir at 45°C for 30 minutes. The stability of the encapsulated pigment dispersion was determined by centrifugation and freeze-thaw methods. Centrifugation method reference. Centrifuge the encapsulated pigment dispersion at 4000 rpm for 60 minutes, then take out 0.03 g of the supernatant in the centrifuge tube and dilute it to 2000 times with distilled water. Then measure the absorbance A of the supernatant by a spectrophotometer.
One method of manufacturing UV-curable inks is to mix a pigment dispersion with monomers, oligomers, photoinitiators, and additives. In many cases, creating a pigment dispersion is the first processing step in manufacturing UV-curable inks and is very important. To process the pigment dispersions of Pigment Red 2 and Pigment Red 122, a dissolver was used for a pre-mixing step followed by a grinding step using a three-roll mill. The components of the dispersions were a monomer/oligomer mixture of acrylates, pigment, and dispersant. The optimal monomer/oligomer mixture of acrylates was determined by the Daniel flow point method. When processing using a three-roll mill, the processing time as well as the final viscosity of the dispersion becomes very important. Each dispersion was passed through the three-roll mill three times and the passing time was recorded to obtain the processing time. To find the correlation between processing time and viscosity, an experimental design was performed for two different pigments. The design of the experimental model was an extreme vertex design type that allows setting upper and lower limits for the input variables.
Based on the experimental design, the expected viscosity and processing time can be estimated. For Pigment Red 2, the model suggested a processing time of 14.47 g/min and a viscosity of 44.58 Pa*s. The actual processing time was 16.46 g/min and a viscosity of 49.10 Pa*s. For Pigment Red 122, the predicted processing time was 24.35 g/min and a viscosity of 43.04 Pa*s. The result was a processing time of 22.98 g/min and a viscosity of 43.80 Pa*s. The use of the Daniel flow point method in combination with the design of experiments can be used to effectively screen the optimum values of monomers/oligomers for new pigments and UV-curable inks. For the experimental design of the Pigment Red 122 dispersion, a mixture design of the extreme vertex type was used. The mixture of monomers/oligomers is a direct result of the optimal mixture found based on the Daniel flow point method for Pigment Red 122. The dispersants used are the polyacrylate dispersants mentioned in Table 4.1. These lower and upper bounds were inserted in Minitab 17, and just like the Pigment Red 2 DOE, the runs were randomized. The degree of the design was set to 2, the same as the DOE for Pigment Red 2. The design space had 13 data points for collecting data. In the simplex design plot, there are 13 blue circles representing the points where data were collected. Processing Time is the variable, with the processing time (in grams per minute) that the pigment was processed in the three-roll mill and the viscosity of the processed dispersion at a shear rate of 50 seconds. The processed dispersion was also checked using a grinder to ensure a high quality dispersion.
Aqueous dispersion of nano-sized CI Pigment Red 122 prepared by ball milling was encapsulated into UV curable resin, 1,6 hexanediol diacrylate (HDDA, monomer) and polyester acrylate (oligomer) using microencapsulation. Encapsulation of the pigment was achieved by mixing the surfactant-stabilized pigment dispersion and the monomer/oligomer microemulsion and subjecting them to microemulsification conditions. Finally, the encapsulated pigment microemulsion film was UV-cured using a water-soluble initiator. Ultracentrifugal sedimentation, scanning electron microscopy and thermogravimetric analysis (TGA) demonstrated effective encapsulation. The stability of the pigment dispersion as well as the encapsulation process were studied. TGA and ultracentrifugal sedimentation results indicate that CI Pigment Red 122 was successfully encapsulated into polyester acrylate/HDDA resin. The oligomer (polyester acrylate) in the presence of the organic pigment stabilizes the microemulsion droplets without the need to introduce any additional hydrophobes (co-stabilizers) in the formulation. Furthermore, the encapsulation efficiency and suspension stability of the microemulsion were optimal when the polyester acrylate/HDDA weight ratio was 3:2. This encapsulation method is actually effective for the modification of organic pigments used in UV-curable inkjet printing inks.
To prepare the nanoscale pigment dispersion, 3.44 g of Pigment Red 122 powder was mixed with 1 mol of SDS (2.8 g) and water until the total weight was 220 g. The mixture was vigorously stirred with a magnetic stirrer for more than 3 h. The resulting mixture was then ball milled with 3 mm glass balls at a ball:powder ratio of 150:1 for 48 h. The ball milled dispersion was then sonicated at 90% amplitude for 1 h with a pulsation rate of 4 s on and 4 s off. The oil phase, consisting of 2 g, 1,6 HDDA (monomer), 3 g of polyester acrylate (oligomer) and a known amount of hydrophobe, was mixed with 0.5 g of SDS dissolved in 35 ml of water. The mixture was stirred for 1 h, and miniemulsions were prepared by ultrasonicating the emulsions at 90% amplitude for 3 min. To these miniemulsions, the prepared nanoscale organic pigment dispersions (5.5 g) were added, pre-sonicated at 90% amplitude for 15 min, stirred for 2 h, and then sonicated at 55% amplitude for 2 min, while the mixtures were mixed with magnetic stirring.
The stability of waterborne nano-pigment red 122 dispersion with styrene-maleic acid copolymer as modifier is greatly affected by additives. The effects of pH value, ionic strength and alcohols on centrifugal stability and temperature stability were studied. The results showed that within the pH range of 7.70-8.96, the pigment 122 dispersion obtained after treatment at different temperatures had high centrifugal stability and small particle size change. The centrifugal stability and temperature stability decreased with the increase of electrolyte concentration, especially AlCl and MgCl. Alcohols had no negative effect on the centrifugal stability and temperature stability of waterborne nano-pigment red 122 dispersion.
NPRD was diluted by half with deionized water and the pH was adjusted with HCl and NaOH to prepare pigment dispersions with different pH values. The Z-average particle size of pigment dispersions with different pH values was measured by sealing a portion of pigment red 122 dispersion in a tube, placing it in an oven and treating it at 50°C for 24 hours, and then measuring the particle size. The other part was sealed in a tube, placed in a refrigerator, treated at -5°C for 24 hours, and then the particle size was measured. Different doses of NaCl, MgCl 2 , AlCl 3 and corresponding deionized water were added to the nano-pigment dispersion and stirred for 30 minutes. The relative absorbance and temperature stability were tested. Different doses of ethanol, diethylene glycol, glycerol and corresponding deionized water were added to the nano-pigment dispersion and stirred for 30 minutes. The relative absorbance and temperature stability were tested.
Reference: [1] Patent: CN106831763, 2017, A, . Location in patent: Paragraph 0033
Reference: [1] Patent: US2005/11403, 2005, A1, . Location in patent: Page 13
Reference: [1] Patent: EP1516896, 2005, A1, . Location in patent: Page/Page column 29
Reference: [1]Patent: CN106831763,2017,A .Location in patent: Paragraph 0033