Research Of The Synthesis And Pigmentation Of Quinacridone And Its Derivative

The present paper relates to the preparation of Quiacridones and Dimethyl succinylsuccinate(DMSS), the influence of the reaction factors, such as solvent,succinate etc. Dimethyl succinylsuccinate(DMSS)is an important intermediate for Quinairdone pigment. In the present dissertation, at a temperature of 100～110℃,by Dieckman reaction, a series of high-quality DMSS were synthesized in the presence of high-boiling solvent using dimethyl succinate(DMS) and sodium methylate as initial materials. By discussing the response of material molar ratio, solvent, reaction temperature, reaction time and sodium alcohol on the impact of product yield, we have got the best reaction conditions :n(DMS): n(sodium methylate) was 1:1.55, the main solvent is xylene and the co-solvent is DMSO , the temperature is 110℃a nd the reaction time is 2～3 hours. Under these conditions, the yield can reach 65.25% . The appearance of DMSS is light gray, after purification, The product structure was confirmed through IR, and its melting point is 154.3～157.6℃.The paper researched the preparing of Pigment Violet 19,C.I Pigment Red 122 and C.I Pigment Red 202. Moreover, the influence of reacting factors, such as solvent, time, temperature etc on the yield, color, shade and other important properties of Quiacridones pigments were studied. Then the factors were finally defined. The concluions of compounding Pigment Violet 19 were drawn as follows: First, n(DMSS): n(Phenylamine) was 1:2.72, the best solvent of condensation reaction is Methyl. And the reaction temperature is the boiling point of solvent lasting 9h. Second, the reaction of oxidizing in the ethanol is better than other organic solvent. The temperature is 78℃lasting 8h. Third, in the ring-closing reaction, the feeding compared to is 1:6, the temperature is 130℃lasting 3h. The reaction yield is 82.0%. The concluions of compounding C.I Pigment Red 122 were drawn as follows: First, n(DMSS): n(Paratoluidine) was 1:2.75, the best solvent of condensation reaction is Methyl. And the reaction temperature is the boiling point of solvent. Second, the method of high pressure is better than in the normal. The temperature in normal is the boiling point of solvent lasting 7h. Third, reaction of oxidizing is in advance, the reaction of oxidizing in the ethanol is better than other organic solvent. The temperature is 78℃lasting 7h. Forth, the reaction of encircling in polyphosphoric acid is better than in dimethylnaphthalene. The feeding compared to is 1:3. The temperature is 110～120℃lasting 4h. The reaction yield is 81.4%. The concluions of compounding C.I Pigment Red 202 were drawn as follows: First, n(DMSS): n(Parachloroaniline) was 1:2.5, the best solvent of condensation reaction is Methyl. And the reaction temperature is the boiling point of solvent lasting 10h. Second, the reaction of oxidizing in the ethanol is better than other organic solvent. The temperature is 78℃lasting 7h. Third, in the ring-closing reaction, the feeding compared to is 1:4, the temperature is 110～120℃lasting 5h. The reaction yield is 81.5%.The paper adopted different conditioning methods, the solvent treatment and using different surface processors, to get the pigmentation of C.I Pigment Red 122 during the synthesis process of pigment (2 steps pigmentation). The influence of the pigmentation factors, such as solvent, time, temperature etc on the color, shade and other important of C.I Pigment Red 122 were studied. Then a kind of conditioning method was found and the factors were finally defined. The pigment was tested by color, shade, transparence, crystal shape etc. According to the test, the pigment has fresh color, good hiding capability and other excellent capabilities. The pigment can compare beauty with the standard sample.