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tosn鐵桿木蟲 (職業(yè)作家)
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[求助]
求翻譯
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求大俠翻譯，見 EXAMPLE 1 This example describes the preparation of diethyl pyrocarbonate with PEG 15 stearamine as the catalyst. A solution of ethyl chloroform ate (114.2 grams(95%) 1.00 mole) and PEG-15 stearamine (1.88 grams (99%) 0.002 mole) was introduce to a 1000 milliliter,three-necked reaction flask with a bottom stopcock. The reaction flask was equipped with a mechanical teflon blade stirrer, sodium hydroxide solution inlet, vent and thermowell for a thermocouple, which was connected to a temperature control unit. Sodium hydroxide was charged to the reaction flask through a Masterflex addition pump. The temperature control unit activated a cooling water pump which directed ice water against the reaction flask and also controlled the Masterflex pump so as to maintain the reaction temperature at below 15° C. When the temperature in the reaction flask was below 15° C., sodium hydroxide solution was charged to the flask. When the temperature rose above 15° C., the Masterflex pump was shut off and ice water sprayed on the reaction flask to cool the contents of the reaction flask. Aqueous sodium hydroxide solution (82 grams (50%) 1.025 moles) was charged to the reaction flask over a period of approximately 60 minutes. Semi-solids which remained on the sides of the flask were rinsed into the liquid reaction mixture with a small amount of water and the reaction mixture post stirred at 15° C. for minutes. 125.5 grams of water (including the amount of rinse water) was added tot he reaction flask so that the theoretical percent solids in the aqueous phase was about 25 percent. The reaction mixture was agitated from 10seconds to dissolve all solids before phase separation was performed. The top organic phase (82.7 grams) was dried over 6.2 grams of magnesium sulfate to give a light yellow clear liquid (77.2 grams). Volatiles in the yellow liquid product were removed by a rotary evaporator under water aspirator vacuum (40 mm/Hg) for 60 minutes at 60° c., and then under vacuum pump (< 2 mrn/Hg) for 60 minutes at 60° C., thereby to obtain a final liquid product (71.8 grams). This product was a clear, light yellow liquid having an APHA color of 100.The conversion of chloroformate to chloride anion (CI-) was found to be 100percent based on the analysis for (CI-) in the aqueous phase. The infrared spectrum of the product matched the literature infrared spectrum for diethyl pyrocarbonate with a characteristic band at 1823em-1. Both 1H (proton) and BC nuclear magnetic resonance analysis supported the product as being diethyl pyrocarbonate with a minor amount of diethyl carbonate. The product has an assay of 96 percent as determined by gas chromatograph analysis 拜托拜托�。�！ |
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2樓2013-04-23 21:48:36
南京工大
木蟲 (小有名氣)
- 翻譯EPI: 14
- 應(yīng)助: 0 (幼兒園)
- 金幣: 1971.3
- 散金: 102
- 紅花: 6
- 帖子: 173
- 在線: 81.1小時(shí)
- 蟲號: 1410020
- 注冊: 2011-09-20
- 性別: GG
- 專業(yè): 高分子組裝與超分子結(jié)構(gòu)
【答案】應(yīng)助回帖
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tosn: 金幣+50, 翻譯EPI+1, ★★★★★最佳答案, xiexi 2013-04-24 22:00:48
tosn: 金幣+50, 翻譯EPI+1, ★★★★★最佳答案, xiexi 2013-04-24 22:00:48
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這一實(shí)例描述了使用硬脂胺聚氧乙烯醚作為催化劑制備焦碳酸二乙酯的過程。氯甲酸乙酯（114.2 g，95%，1 mol）溶液和硬脂胺聚氧乙烯醚（1.88 g，99%，0.002 mol）加入到底部帶有活塞的1000毫升的三口燒瓶中。燒瓶配有一個(gè)特氟龍材質(zhì)的槳式攪拌器，一個(gè)氫氧化鈉溶液的加入口和出口，以及一個(gè)套管用于安裝熱電偶，熱電偶接在控溫裝置上。氫氧化鈉溶液通過Masterflex蠕動(dòng)泵滴加入反應(yīng)體系�？販匮b置與一個(gè)冷卻水泵相連，可以控制冰水的流出以冷卻反應(yīng)裝置，還可以控制蠕動(dòng)泵的流速以使得反應(yīng)溫度在15°C以下。 當(dāng)反應(yīng)裝置中的溫度在15°C以下時(shí)，氫氧化鈉溶液就被加入到燒瓶中。當(dāng)溫度升高到15°C以上時(shí)，蠕動(dòng)泵停止工作，冰水被噴射到反應(yīng)裝置上以降低反應(yīng)物溫度。 氫氧化鈉溶液（82 g，50%，1.025 mol）應(yīng)在60分鐘左右的時(shí)間內(nèi)被加入到反應(yīng)裝置中。反應(yīng)結(jié)束后，粘在燒瓶壁上的少量半固體物質(zhì)可以用少量的水沖洗到液相反應(yīng)混合物中，并保持在15°C下繼續(xù)攪拌幾分鐘。向裝置中加入125.5 g水（含沖洗所用的水），這樣液相中理論的固含量即為25%。在相分離現(xiàn)象發(fā)生前，搖晃反應(yīng)混合物約10秒鐘以使得所有固體溶解。 使用6.2g無水硫酸鎂對上層的有機(jī)相（82.7 g）進(jìn)行脫水，得到了淺黃色的清澈液體（77.2 g）。該液體中的易揮發(fā)組分通過使用旋轉(zhuǎn)蒸發(fā)儀，先在水泵抽真空條件（40 mm/Hg）下60°C旋轉(zhuǎn)蒸發(fā)60分鐘，接著再在真空泵作用下（<2 mm/Hg）60°C旋轉(zhuǎn)蒸發(fā)60分鐘除去，最終得到液相的產(chǎn)物（71.8 g）。該產(chǎn)物為淡黃色的清澈液體，色度為100。通過對液相產(chǎn)物的分析可知，氯甲酸酯中的氯元素的轉(zhuǎn)化率為100%。產(chǎn)物的紅外光譜與文獻(xiàn)中焦碳酸二乙酯的光譜一致，在1823 em-1處有特征峰。1H和BC的核磁共振分析都證實(shí)了該產(chǎn)物為焦碳酸二乙酯，其中含有很少量的碳酸二乙酯。通過氣相色譜分析，該產(chǎn)物的含量為96%。 |
3樓2013-04-23 22:16:21
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