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It can be used as raw material and organic intermediate of pharmacy, and also as solvent; It can be used as analytical reagent and extractant of aluminum in tungsten and molybdenum; Pentanedione, also known as acetylacetone, is a bactericide methylthiamine, the intermediate of thiamine and herbicide thiosulfuron.; Acetylacetone is an intermediate of organic synthesis, which forms ammonia with guanidine..
Different process routes can be adopted: reaction between acetone and ethenone or condensation between acetic anhydride and acetone or condensation between acetone and ethyl acetate. The reaction process between acetone and ethenone actually takes acetone as the raw material, through ethenone, isopropylene acetate, and then through conversion to obtain acetylacetone process is as follows: the acetone containing 1/1000 carbon disulfide is vaporized and then introduced into a cracking furnace of 780-800 ℃ to generate ethenone (or glacial acetic acid is vaporized by triethyl phosphate catalyst, using ammonia as stabilizer, after cracking in a cracking furnace at 700 ℃ to ethenone), ethenone is absorbed by acetone. In the presence of sulfuric acid or acetyl sulfonyl, it reacts with acetic acid at 61-71 ℃ to form isopropylene acetate. After distillation and purification, the purity of isopropyl acetate can reach more than 93-95. Then, isopropylene acetate is vaporized, preheated to 560-570 ℃ conversion furnace is introduced, acetylacetone is generated through intramolecular rearrangement, and the finished product is purified by condensation and fractional distillation. Each ton of product consumes about 2700kg of acetone. The condensation process between acetone and ethyl acetate is carried out in the presence of sodium metal. Operation example 1 add 120ml of refined ethyl acetate and 32ml of ammonia to the cooled beaker. After adding sodium Amino, shake it in ice water for 24 hours and leave it overnight at room temperature. Add 100g ice the next day, then add the same amount of ice water, take the water layer, and add dilute sulfuric acid to make it acidic. In this solution, add saturated copper (II) acetate solution (dissolve 40g of powdered copper (II) acetate with a certain amount of hot water) to make acetylacetone form copper salt precipitation. If the reaction solution is alkaline, a small amount of acetic acid can be added. After 2-3 hours, filter the blue-gray acetylacetone and wash it twice with water, Move directly into separating funnel, add ether to shake continuously, and add 50ml4N sulfuric acid to decompose it. Take ether solution, then extract acetylacetone from acid layer with ether, combine ether solution twice, and dry with calcium chloride. The ether was distilled off and the residue was continued to be distilled, and the 125-140 °c fraction was collected. Then the essence is retained at 135-140 ℃, and the yield is about 15-20g. Boiling point 139 ℃. Operation example 2 in a 1500ml round bottom flask, 25g of sodium metal and 20ml of diethyl ether were added, and then 225ml of ethyl acetate cooled with coolant was added. Add 73ml of acetone with cooling and constant stirring. Place at room temperature for 4 hours, add 400ml of water, separate the ethyl acetate in the water layer, neutralize the water layer with acetic acid, and then add copper (II) acetate solution (125g copper (II) acetate dissolved in 1500ml of water) to form green acetylacetone chelate. After 2-3 hours, the precipitation was complete and filtered. The precipitate was suspended in ether, shaken with 50ml of 40 dilute sulfuric acid, and the ether layer was dried with calcium chloride. Steam away the ether, fractionate the remaining oil, collect the 124-140 °c fraction, and then fractionate, and collect the 139-140 °c fraction. The condensation reaction between acetic anhydride and acetone is carried out under the catalysis of boron trifluoride, and the yield of this method is relatively high. Refining method of acetylacetone: dissolve about 20ml of crude acetylacetone in 80ml of benzene, and then oscillate with isometric distilled water for 3 hours. Acetic acid which is soluble in water is distributed into the aqueous phase, while acetylacetone is easily soluble in benzene. Acetylacetone in benzene phase can be directly applied or benzene can be distilled. Raw material consumption quota: acetone (industrial products, Water content <0.5)2553 kg/t; Fuming sulfuric acid (calculated as h2s04) 12 kg/t; Acetic anhydride (95)19 kg/t; Carbon disulfide (chemical purity) 6 kg/t.
S21: smoking is not allowed during use.
S23: do not breathe in steam.
S24/25: prevent contact between skin and eyes.
R10: flammable. R22: swallowing is harmful.
UN2310
GHS02,GHS06
The warehouse is ventilated cryodrying and stored separately from the oxidant.
P261;P280;P311
III
Danger
H226;H302;H311;H331
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