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Laboratory method for making adipic acid in the optimum amount of potassium permanganate

Skills, we give students experience in open loop feast, that is prepared by chromic acid oxidation of cyclohexanone. And then obtained their raw materials for cyclohexanone. Potassium permanganate oxidation in weak alkaline conditions in the system of adipic acid, saving the raw materials. And train the students conscientious and careful scientific approach to experiment. Preparation of adipic acid reaction principle: / - a Fol ' = 0-Z - ~ HOOC (CH2)' COOH - / l in the experimental part of the thermometer with an electric mixer and three 250ml neck flask, add 5ml cyclohexanone, 7 grams of sodium carbonate and 5Oral distilled water. Start the blender, stirring rapidly under the conditions. Every 2 - 4 minutes by adding a small amount of research small batches of potassium permanganate,[link widoczny dla zalogowanych], the amount was 13 grams, 11 grams, l5 g, l6 g, I7 grams. Beginning with a water bath heated to the reaction solution temperature was 28 - 30_c. And maintained at this temperature range. After adding potassium permanganate will continue after the mixing. Until the rise in temperature until the reaction solution. And then heated in 50C water bath for half an hour, continue stirring. At this point, the amount of reaction will be too precipitate manganese dioxide fE. Filter paper in a flat. Point drop of the mixture, testing reaction completion + as observed in the test solution with purple exist, then used a small amount of solid sodium bisulfite to Chen out excess potassium permanganate. Hot filtration. With 20m] 10 of the sodium carbonate solution washing residues. While stirring, slowly dropping concentrated sulfuric acid. Until the filtrate was strongly acidic. Carefully heat the filtrate evaporated. The filtrate volume reduced to 25m1. Then cool. White monoclinic materials with adipic acid Xin out of the body. Filtration, dried, weighed. 2 Results and discussion results from the following Lingge (see next page) shows that: ho Date received: 1 ∞ s-O3-2O Bu Table l potassium permanganate oxidation of cyclohexanone from 5ml had two Bu yield (g) 1. Potassium permanganate dosage 16g, l7g time, that is, 0.101mol, 0.108mnl, the highest yield of adipic acid, but the rejection of 17g of potassium permanganate, the use a certain amount of sodium bisulfite to remove excess potassium permanganate, but with 16g potassium permanganate, as long as the amount of used sodium bisulfite step to remove the excess potassium permanganate. 2. Thus, cyclohexanone and potassium permanganate reaction principle is: / a Na, co = 0 +2 KMnOd-KOOC (CH2). COOK +2 MnO2 + H2O -_/KOOC (CH2) 4COOK + HO. = HOOC (CH2) 4COOH + K2SO. The theory of Cyclohexanone with potassium permanganate according lmol: 2mol amount of the reaction, in fact, 1:2.0 l for the molar volume, the effect is good, the best yield, the amount of sodium bisulfite the least.