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John126
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上文中"the metering mixture"應(yīng)該是指100 g and 84 g of hydroxyacetone paraldehyde are mixed，這兩個(gè)物質(zhì)在19-21℃混合。將此混合物慢慢加到預(yù)先加熱至50℃的混合物中（27 g of concentrated hydrochloric acid, 33 g of water and 2.5 g of tetrabutylammonium bromide solution., 50 wt .-% in water, are combined ），滴加時(shí)間7小時(shí) |
4樓2015-12-17 09:59:37
John126
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【答案】應(yīng)助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
感謝參與，應(yīng)助指數(shù) +1
wu_bing: 金幣+30, ★有幫助, 謝謝 2015-12-18 09:45:00
感謝參與，應(yīng)助指數(shù) +1
wu_bing: 金幣+30, ★有幫助, 謝謝 2015-12-18 09:45:00
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Example 1 Preparation of 2,3-pentanedione on a Laboratory Scale Preparation of the metering: 100 g and 84 g of hydroxyacetone paraldehyde are mixed. Carrying • guidance of the reaction: 27 g of concentrated hydrochloric acid, 33 g of water and 2.5 g of tetrabutylammonium bromide solution., 50 wt .-% in water, are combined and heated to 50 ° C. At this temperature the metering mixture (temperature metering mixture: 19-21 ° C) were added within 7 hours. Then a further 38 g water are added to the reaction mixture and a mixture which consists of water and 2,3-pentanedione substantially distilled off at atmospheric pressure. Subsequently, the phases are separated. This gives 125 g • old 2,3-pentanedione, 92 wt .-% pure according to gas chromatogram. This corresponds to a yield of 85% of the starting material used in deficit. Example 2 Preparation of 2,3-pentanedione on the industrial scale production of the metering: 150 kg and 126 kg hydroxyacetone paraldehyde are mixed. Carrying • guidance of the reaction: 40 kg of concentrated hydrochloric acid, 50 kg of water and 4 kg of tetrabutylammonium bromide solution., 50 wt .-% in water, are successively in the reactor GEF • filled and heated to 50 ° C. At this temperature the metering mixture (temperature metering mixture: 10 ° C.) is metered within 10 hours. A further 60 kg of water are added to the reaction mixture and a water / 2,3-pentanedione mixture is distilled off at atmospheric pressure. Subsequently, the phases are separated. This gives old • 174 kg of 2,3-pentanedione, 94 wt .-% pure according to gas chromatogram. This corresponds to a yield of 81% of the starting material used in deficit. |
2樓2015-12-15 09:33:45
3樓2015-12-15 09:58:40
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5樓2015-12-17 10:56:21
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