Preparing method of pigment red 122
A pigment red and solvent technology, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve the problems of increased environmental protection treatment costs, high production costs, and difficulty in recycling, and achieves reduction of environmental protection treatment costs, difficulty in recycling, and other problems. The effect of reducing production costs
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Embodiment 1
[0034] (1) Preparation of intermediate DTTA: In a pressure reactor, add 250g of methanol and 43.2g of p-toluidine in sequence. After stirring and dissolving, add 10g of 31% hydrochloric acid and 41g of DMSS, heat to 100°C, keep the temperature for 4 hours, and then cool down to 60°C, add 60g of 50% NaOH, heat to 110°C, pass air into the reaction kettle, the flow rate is 4 liters per hour, after oxidation for 8 hours, add 300g of water to dilute, after stirring for 1 hour, filter to remove slag, add the filtrate Acidify with 16% dilute hydrochloric acid, adjust PH=5, precipitate DTTA purple crystals, filter again (filtrate collection and detection), wash the filter cake to neutrality, and dry to obtain 62.4g of DTTA, the yield is 93.69%, liquid chromatography analysis The purity is 96.42%, and the spectrum is as follows figure 1 As shown, wherein, DTTA liquid chromatography detection conditions: mobile phase composition is acetonitrile-ammonium acetate buffer (PH=4.0), volume r...
Embodiment 2
[0039] (1) Preparation of intermediate DTTA: In a pressure reactor, add 300g of n-butanol and 50.1g of p-toluidine in sequence. After stirring and dissolving, add 12g of 31% hydrochloric acid and 36g of DMSS, heat to 80°C, and keep it warm for 3 hours. Cool down to 60°C, add 75g of 50% NaOH, heat to 95°C, pass air into the reaction kettle with a flow rate of 7 liters for an hour, after oxidizing for 6 hours, add 300g of water to dilute, stir for 1 hour, filter to remove slag, The filtrate was acidified with 30% sulfuric acid, adjusted to PH = 3, DTTA purple crystals were precipitated, filtered again (filtrate collection and detection), the filter cake was washed to neutral, and dried to obtain 63.6g of DTTA with a yield of 95.50%. Phase chromatogram such as image 3 Shown, wherein, the analytical purity of product DTTA is 96.79%:
[0040] The specific data are shown in Table 2:
[0041] name
[0042] (2) Preparation of Pigment Red 122: In a three-neck flask, add 35...
Embodiment 3
[0044] (1) Preparation of intermediate DTTA: In a pressure reactor, add 350g of isopropanol and 54.4g of p-toluidine in sequence. After stirring and dissolving, add 15g of 31% hydrochloric acid and 54g of DMSS, heat to 110°C, and keep it warm for 5 hours. Cool down to 60°C, add 90g of 50% NaOH, heat to 110°C, pass air into the reaction kettle with a flow rate of 10 liters for an hour, oxidize for 8 hours, add 300g of water to dilute, stir for 1 hour, filter to remove the slag, The filtrate was acidified by adding 16% dilute hydrochloric acid, adjusted to PH=4, DTTA purple crystals were precipitated, filtered again (filtrate collection and detection), the filter cake was washed to neutrality, and dried to obtain 64.1g of DTTA, with a yield of 96.24%. The liquid chromatogram is as Figure 5 Shown, wherein, the liquid chromatography analysis purity of product DTTA is 96.07%, and concrete data is as shown in table 3:
[0045] table 3:
[0046]
[0047]Prepare Pigment Red 122:...
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