Process for preparing DPP pigment
A technology of pigments and surfactants, applied in the field of preparation of DPP pigments, can solve the problems of pigment application limitations, by-products are difficult to remove, etc., and achieve the effects of improving application performance, increasing yield, and improving safety
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Embodiment 1
[0034] 1. Synthesis of crude pigments
[0035]Mix 4.66g (0.2mol) sodium with 95.2ml tert-amyl alcohol, heat to melt the sodium, then start stirring to completely dissolve the sodium in tert-amyl alcohol to generate sodium tert-amyl alcohol, add 13.8g (0.13mol) benzonitrile and 14.2g (0.07mol) diisopropyl succinate, heated to reflux in a nitrogen atmosphere, kept warm for 6 hours, cooled to 90°C, poured into 200g water / methanol (water / methanol=1 / 1 weight ratio ), then heated up to 50°C, kept for 2 hours, cooled to room temperature, filtered, washed with water until neutral, and dried to obtain 14.5g (0.10mol) of a red solid with a yield of 74.9%. This is a crude pigment.
[0036] 1. Solvent treatment
[0037] Put 26.7g of crude pigment into 530ml of N-methylpyrrolidone and heat to reflux for 6 hours. After reflux, cool to 50°C and filter. After the filter cake is pressed dry, it is washed with water until there is no solvent, and 51.3g of wet product is obtained. (water conte...
Embodiment 2
[0041] 1. Synthesis of crude pigments
[0042] Mix 4.66g (0.2mol) sodium with 95.2ml tert-amyl alcohol, heat to melt the sodium, then completely dissolve the sodium in tert-amyl alcohol under stirring to generate sodium tert-amyl alcohol, add 18.3g (0.13mol ) p-chlorobenzonitrile and 18.5g (0.07mol) diisoamyl succinate, heated up to reflux in a nitrogen atmosphere, kept the temperature for 6 hours, cooled to 90°C, poured 200g of water / methanol (water / Methanol=1 / 1 weight ratio), then be warming up to 50 ℃, keep 2 hours, cool to room temperature, filter, wash with water to neutrality, obtain 25.5g (0.10mol) red solid after filter cake drying, yield 78% , which is crude pigment.
[0043] 2. Solvent treatment
[0044] Put 30g of pigment crude product into 500ml quinoline and heat to reflux, keep for 5 hours, cool to 50°C after reflux and filter, press dry and wash with water until solvent-free, obtain 58.3g wet product (water content 51.3%), collect The yield is 94.6%. This is...
Embodiment 3
[0048] 1. Synthesis of crude pigments
[0049] Mix 4.66g (0.2mol) of sodium with 95.2ml of tert-amyl alcohol, heat to melt the sodium, and then completely dissolve the sodium in tert-amyl alcohol under stirring to generate sodium tert-amyl alcohol, add 23.8g (0.13mol) 4-cyanobiphenyl and 21.0g (0.07mol) cyclohexyl succinate, heated up to reflux in a nitrogen atmosphere, kept the temperature for 6 hours, cooled to 90°C, poured 200g of water / methanol (water / methanol =1 / 1 weight ratio), then warming up to 50°C, keeping for 2 hours, cooling to room temperature, filtering, washing with water until neutral, and drying the filter cake to obtain 22.5g (0.10mol) red solid, yield 80%, This is crude pigment.
[0050] 2. Solvent treatment
[0051] Put 30g of the crude pigment into 500ml of N,N-diethylformamide and heat it to reflux for 5 hours. After the reflux, cool to 50°C and filter. After the filter cake is pressed dry, it is washed with water until there is no solvent, and 58.3g of...
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