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xubei9558金蟲 (小有名氣)
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[求助]
鈀炭的回收
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| 本人正在做鈀炭的回收試驗，只能回收85%，含量也只有98%，資料上可以回收95%，含量也可以達到99.95%。但就是做不到，誰有回收鈀炭的工藝，必重謝！ |
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5樓2011-06-16 20:01:36
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xubei9558(金幣+1): 謝謝 2011-06-15 09:43:56
3樓2011-06-14 21:05:41
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xubei9558(金幣+1, 博學EPI+1): 謝謝了 2011-06-15 09:41:09
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一、鈀炭的回收： 1. 無水乙醇中回流30分鐘以上； 2. 乙醇－水（2:1）混合溶劑中回流30分鐘以上。過濾，濾液如不澄清，需重新回流。 二、鈀炭的制備： 5%的鈀碳的做法：把氯化鈀溶解在鹽酸里，一定要溶解澄清透明，鹽酸的量可以自己定，一般溶解清楚透明就可以了，活性炭要選擇，不要顆粒太粗，200目以上就可以了，普通的活性碳要篩。然后把水加熱到60～70℃，一定要去離子水。然后在10～15分鐘內(nèi)把氯化鈀滴加到水里， 加完后再攪拌2小時左右，然后用甲醛中和到溶液到中性。然后冷卻過濾，或者熱過濾都沒有關(guān)系，過濾后用去離子水洗掉氯離子，一般用氯化銀來檢查，一般做10克鈀碳用400克水加熱滴定，要注意，5%的鈀碳是以鈀金屬來算，不是氯化鈀來算，其他含量的做法錯不多，處理氯化鈀活性碳的粒度，越細越好，你還可以把活性碳用酒精處理一下再用。 鈀／炭催化劑(5％Pd) 將優(yōu)質(zhì)活性炭用l0％硝酸在蒸氣浴上加熱2—3h、用水 洗滌硝酸，在l00—ll0℃烘干。取93克處理過的活性炭懸浮在 1．2升水中，加熱至80℃，在此懸浮液中，加入8．2克(o．046摩 爾)氯化把溶于20毫升濃鹽酸相50毫升水的溶液。在快速攪拌下 加入8毫升(o．1摩爾)37％甲醛溶滄。保持恒定攪拌，加30％ 氫氧化創(chuàng)溶液使懸浮液對石蕊試紙稍呈堿性。繼續(xù)攪拌5分鐘。 過濾，用每份250毫升水洗滌10次。盡可能抽吸至于。濾塊先在室 溫下空氣中晾干，然后在有氫氧化部(或氯化鈣)的干燥器中干 燥。得干燥催化劑92—98克。在密閉瓶中保存。 鈀／炭催化劑(10％Pd) 在蒸氣浴上加熱8．33克氯化把在5．5毫升濃鹽酸和40毫升水 中的混合物使成溶液，加到盛有135克醋酸鈉三水合物在500毫升 水的溶液的1升還原瓶中。加入55克優(yōu)質(zhì)活性炭。通氫到混合物 中至1—2小時后不再吸收為止。用布氏漏斗過濾，用2L水分 五次洗滌。除去大部分水的濾塊先在空氣中晾干，然后在有氯化 鈣的干燥器中干燥。得催化劑40～50克，粉碎后貯存在密閉瓶中。 這是有機制備化學手冊中的制法，比較經(jīng)典，應(yīng)該可以 參考文獻： Org．Syn．， Coll．V0l．3, PP 685(1955) A. Palladium on barium sulfate catalyst (5% Pd). A solution of 8.2 g. of palladium chloride (0.046 mole) in 20 ml. (0.24 mole) of concentrated hydrochloric acid and 50 ml. of water is prepared. To a rapidly stirred, hot (80°) solution of 126.2 g. (0.4 mole) of reagent barium hydroxide octahydrate in 1.2 l. of distilled water contained in a 4-l. beaker and is added all at once 120 ml. (0.36 mole) of 6 N sulfuric acid. More 6 N sulfuric acid is added to make the suspension just acid to litmus. To this hot barium sulfate suspension are added the palladium solution and 8 ml. (0.1 mole) of 37% formaldehyde solution. The suspension is then made slightly alkaline to litmus with 30% sodium hydroxide solution, constant stirring being maintained. The suspension is stirred 5 minutes longer, and then the catalyst is allowed to settle . The clear supernatant liquid is decanted and replaced by water, and the catalyst is resuspended. The catalyst is washed by decantation eight to ten times. After the final decantation, the catalyst is collected on a 90-mm. medium-porosity sintered-glass funnel. Most of the water is removed from the cake, but not enough to cause the cake to break or channel. The filter cake is washed with 250 ml. of water in five portions, the last being removed as completely as possible by filtration. The funnel and its contents are then placed in an oven at 80° until the catalyst is dry. The catalyst (93–98 g.) is powdered and stored in a tightly closed bottle. B. Palladium on carbon catalyst (5% Pd). A suspension of 93 g. of nitric acid-washed Darco G-60 in 1.2 l. of water contained in a 4-l. beaker and is heated to 80°. To this is added a solution of 8.2 g. (0.046 mole) of palladium chloride in 20 ml. (0.24 mole) of concentrated hydrochloric acid and 50 ml. of water . Eight milliliters (0.1 mole) of 37% formaldehyde solution is added. The suspension is made slightly alkaline to litmus with 30% sodium hydroxide solution, constant stirring being maintained. The suspension is stirred 5 minutes longer. The catalyst is collected on a filter and washed ten times with 250-ml. portions of water. After removal of as much water as possible by filtration, the filter cake is dried, first in air at room temperature, and then over potassium hydroxide in a desiccator. The dry catalyst (93–98 g.) is stored in a tightly closed bottle. Organic Syntheses, CV 3, 685 |
4樓2011-06-14 21:13:28
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