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quinacridone/naphthalene sulfonic acid formaldehyde polymer[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 mi concentrated (95-98%) sulfuric acid. 31.2 G unsubstituted quinacridone (CROMOPHTALS RED 2020, Ciba Specialty Chemicals Inc.) is added at a temperature below 45C and the mixture is stirred for 10 minutes at 40-45C to dissolve the pigment. 39.7 G of a wet naphthalene SULFONIC acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% <strong>[532-02-5]2-naphthalene sulfonic acid sodium salt</strong> (Shanghai Shen Li Chemical Factory) is added at a temperature below 45C and the mixture is stirred for 15 minutes at 40 to 45C followed by the rapid addition of 3.2 G para formaldehyde. The reaction mixture is stirred for one hour at 58-60C, then poured into 2.5 I of ice water. The violet precipitate is stirred for 1 hour at 5-20 C, then filtered. The residue is washed with water to a pH of 2.5 and kept as presscake with a solid content of 13% by weight. Around 0. 5 G of the press cake are reslurried in 20 mi hot water yielding a bluish red colored liquid. It is filtered to remove little aggregated material. The filtrate is red and appears a dye solution. However, the electron micrograph shows the quinacridone in nanosize particle form with an average particle size of 4 to 25 nm.
poly(formaldehyde-co-1-naphtalene sulfonic acid sodium salt-co-2-naphtalene sulfonic acid sodium salt); quinacridone; naphtalene sulfonic acid methyl metacridone; mixture of[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
A one liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 ml concentrated (95-98%) sulfuric acid. 31.2 G unsubstituted quinacridone (CROMOPHTALO Red 2020, Ciba Specialty Chemicals Inc.) are added at a temperature BELOW 45C and the mixture is stirred for 10 minutes at 40-45C to dissolve the pigment. 39.7 G of a wet naphthalene sulfonic acid sodium SALT PRESSCAKE with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene SULFONIC acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature below 45C and the mixture is stirred for 15 minutes at 40-45C followed by the rapid addition of 3.2 G para formaldehyde. The reaction mixture is stirred for one hour at 58-60C then poured into 2. 5 1 ice water. The violet precipitate is stirred for 1 hours at 5-20C, then filtered. The violet press cake is washed with water to a pH of about 2.5 and kept as presscake. About 0.5 G of the press cake are RESLURRIED in 20 mi hot water yielding a red colored liquid which is filtered through paper to remove little aggregated material. The filtrate is red and appears like a dye solution. However, the electron micrograph shows the quinacridone in nanosize particle form with an average particle size of 4 to 25 nm. A small sample of the violet presscake is further washed to a pH of 5 and dried and analytically tested by MALDI. When measured in positive mode, it shows as main component quinacridone (m/z 314 peak), and only a trace of naphthalene SULFONIC acid methyl quinacridone (m/z 535 peak) is found as shown in Figure 1. When measured in negative mode, again the quinacridone is visible (m/z 312 peak) and the polymeric structure of the naphthalene sulfonic acid-formaldehyde polymer is clearly visible with the main molecular weight peaks at 428,649, 870,1091, 1312, 1534,1755 and 1976. The negative mode MALDI spectrum is shown in Figure 2.
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