| 340 kg |
|
In the diazo pot by adding 1000 kg water and 160kg30% hydrochloric acid, is added under agitation giving cash 150kg3-amino-4-methoxy compositions, beating 1 hours, with ice-cooling to 0 C the following, adjusting volume to 2500L, dissolved in advance of to 40% of the content of sodium nitrite (folding stem 42.5 kg sodium nitrite water 64 kg), measured end point keep the potassium iodide starch paper micro-blue, keeping temperature 5-10C, stirring 30 minutes, add 20 kg of diatomaceous earth, stirring 20 minutes, filtered salt solution.A small quantity of water of added to the coupling pot, open stirring, will giving cash 186.5kg5 - (2 the [...] -hydroxy -3 the [...] -naphthalene carboxamide yl) - 2-benzimidazolone adding the colloid rubs into randoms pot, by adding 0.6 kg eighteen alkane mellow base polyoxyethylene ether, beating 0.5 hours, adjusting volume to 1500L, adjusting temperature is 0-10C.The diazonium salt is slowly added to the pulping solution of 5 - (2 the [...] -hydroxy -3 the [...] -naphthalene carboxamide yl) - 2-benzimidazolone suspension coupling reaction in, at the same time, in the coupling process the mass concentration 20% of sodium bicarbonate solution dripped into randoms pan, maintain the reaction system pH value is 5.5-6.0, coupling component dropping time is 0.5-1 hours, randoms temperature 5-10C, randoms end, re-stirring and a half hours, heating to 70-80C, thermal insulation 1-2 hours, the invention aims to, rinse resulting pigment after the coarse filter.Added to the reaction kettle pyrrole winds the alkane alkone 2000L, adding the above-mentioned pigment crude, beating, raising the temperature to 100-110C, thermal insulation 2 hours, specifically pigment conversion situation, cooling to 40-50C, filtering, washing, 80 C drying, crushing C.I is obtained. Pigment red 176 finished product. Number is about 340 kg. |
|
|
27 parts of the compound (b-3) and 96 parts of a 25% sodium hydroxide aqueous solution were dissolved in 208 parts of methanol to prepare a coupler solution. On the other hand, 20 parts of the compound (a-1) was dispersed in 320 parts of water, ice was added to adjust the temperature to 5 C., 36.3 parts of a 35% hydrochloric acid aqueous solution was added and stirred for 1 hour and then sodium nitrite Was added to 19.2 parts of water to prepare an aqueous solution, and the mixture was stirred for 2 hours. An aqueous solution comprising 93 parts of 80% acetic acid aqueous solution, 106 parts of 25% sodium hydroxide aqueous solution and 112 parts of water was added to prepare an aqueous diazonium salt solution.The coupler solution was injected into the aqueous solution of diazonium salt at 5 C. over 30 minutes to carry out a coupling reaction. After stirring for 2 hours, after disappearance of the diazonium salt was confirmed, it was heated to 60 C., Filtered, washed with water, and dried at 80 C. for 24 hours to obtain 45 parts of the pigment represented by the formula (5). 5 parts of the pigment of the formula (5) was crushed into 100 parts of 98% sulfuric acid and charged at 15 C. or less.Thereafter, the temperature was raised to 60 C., stirred for 2 hours, and slowly added dropwise to 2,000 parts of cold acetone prepared separately. The precipitate was filtered, washed twice with 1000 parts of cold acetone, and dried at 80 C. for 24 hoursAnd dried for 6.1 parts of a red compound. As a result of mass spectrometric analysis by LC-MS, it was identified that the following compound (A-3) was the main component. |
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
