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管道化重氮化翻譯實(shí)例4
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EXAMPLE 4 Diazotization of Aniline in a Cross-Flow Recycle Reactor 9.11 kg (97.96 g-moles) of aniline was added with stirring to 11.77 kg (588.5 g-moles) of HF in tank 34 while maintaining a temperature of 5.degree. C. via cooling water, thereby forming a solution of aniline-HF at a 1 to 6 molar ratio. Then 6.76 kg (97.97 g-moles) of sodium nitrite were added with stirring to 23.51 kg (1173 g-moles) of HF in tank 36 while maintaining a temperature of 2.degree. C. via cooling water, thereby forming a solution of nitrosyl fluoride in HF at a 1 to 12 molar ratio. The aniline-HF solution was fed continuously to the multi-stage reactor for one hour at 25.degree. C. at a flow rate of 200 ml/min. Once the multi-stage reactor was filled with aniline-HF the recycle pump 64 was set to deliver 2,050 ml/min. or a 4.81 mass ratio of recycled to total mass in. The nitrosyl fluoride-HF solution was injected incrementally into lines 38, 44 and 48 immediately prior to each of the three static mixers. The proportions of nitrosyl fluoride fed to static mixer 58, 74 and 68 respectively, were 50%, 40% and 10%. The nitrosyl fluoride solution was fed continuously for one hour at 10.degree. C. by pressurizing tank 36 and controlling the flow rate at 209 ml/min. via a control valve (not shown) allowing approximately 7% of the feed aniline to exit at 70 unconverted. The temperature of the reaction mixture was maintained by pumping a solution of glycol and water, maintained at 5.degree. C. by a chiller, through heat exchangers 60 and 62. The cooling solution flow was maintained such that the temperature of the reaction mixture was between 5 and 25.degree. C. in the first two reaction sections and between 5 and 18.degree. C. in the third reaction section. The completely reacted reaction mixture leaving the recycle reactor was a clear brownish-orange solution that was collected for further processing to produce fluorobezene. Test samples of the reaction mixture were collected every five minutes. Of the samples taken, the concentration of benzene diazonium fluoride was between 2.59 g-mole/liter and 2.61 g-mole/liter, corresponding to a conversion of between 98% and 100% of aniline to benzene diazonium fluoride, based on nitrosyl fluoride injected. |

木蟲之王 (文壇精英)
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EXAMPLE 4 示例4 Diazotization of Aniline in a Cross-Flow Recycle Reactor 在錯(cuò)流循環(huán)反應(yīng)器中苯胺的重氮化 9.11 kg (97.96 g-moles) of aniline was added with stirring to 11.77 kg (588.5 g-moles) of HF in tank 34 while maintaining a temperature of 5.degree. C. via cooling water, thereby forming a solution of aniline-HF at a 1 to 6 molar ratio. 在通入冷卻水保持5℃、已有11.77公斤(588.5摩爾)HF的反應(yīng)罐34中,伴隨攪拌加入9.11公斤(97.96摩爾)苯胺,從而形成了摩爾比在1至6的苯胺-HF溶液。 |

木蟲之王 (文壇精英)
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Then 6.76 kg (97.97 g-moles) of sodium nitrite were added with stirring to kg (1173 g-moles) of HF in tank 36 while maintaining a temperature of 2.degree. C. via cooling water, thereby forming a solution of nitrosyl fluoride in HF at a 1 to 12 molar ratio. 在通入冷卻水保持2℃、內(nèi)有23.51公斤(1173摩爾)HF的反應(yīng)罐36中,攪拌下加入6.76公斤(97.97摩爾)亞硝酸鈉,從而在HF中形成了摩爾比在1至12的亞硝基氟溶液。 The aniline-HF solution was fed continuously to the multi-stage reactor for one hour at 25.degree. C. at a flow rate of 200 ml/min. 苯胺- HF溶液連續(xù)輸送到25℃的多級(jí)反應(yīng)器,時(shí)間為一小時(shí),流速為200毫升/分鐘。 |

木蟲之王 (文壇精英)
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苯胺- HF溶液連續(xù)輸送到25℃的多級(jí)反應(yīng)器,時(shí)間為一小時(shí),流速為200毫升/分鐘。 Once the multi-stage reactor was filled with aniline-HF the recycle pump 64 was set to deliver 2,050 ml/min. or a 4.81 mass ratio of recycled to total mass in. 一旦苯胺HF充滿了多級(jí)反應(yīng)器,循環(huán)泵64被設(shè)置為2,050毫升/分鐘,或按總質(zhì)量循環(huán),其質(zhì)量比為4.81。 The nitrosyl fluoride-HF solution was injected incrementally into lines 38, 44 and 48 immediately prior to each of the three static mixers. 把亞硝基氟-HF溶液依次注入三個(gè)靜態(tài)混合器前的管線38、44和48。 The proportions of nitrosyl fluoride fed to static mixer 58, 74 and 68 respectively, were 50%, 40% and 10%. 按50%、40%和10%的比例將亞硝基氟分別輸送到靜態(tài)混合器58、74和68。 The nitrosyl fluoride solution was fed continuously for one hour at 10.degree. C. by pressurizing tank 36 and controlling the flow rate at 209 ml/min. via a control valve (not shown) allowing approximately 7% of the feed aniline to exit at 70 unconverted. 把亞硝基氟溶液用一小時(shí)在10℃連續(xù)輸送,通過(guò)密封罐36中,且流速控制在209毫升/分鐘,是通過(guò)控制閥(未顯示),使大約7%的苯胺進(jìn)料輸出(未轉(zhuǎn)化的)70。 |

木蟲之王 (文壇精英)
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反應(yīng)混合物方案溫度的維持是由泵入經(jīng)由冷卻器5℃的乙二醇和水的溶液,通過(guò)了熱交換器60和62。 保持冷卻的溶液的流量,這樣在前兩個(gè)反應(yīng)階段中反應(yīng)混合物的溫度在5至25℃,第三反應(yīng)階段在5和18℃之間。 流出循環(huán)反應(yīng)器的完全反應(yīng)的反應(yīng)混合物是淡的棕橙色溶液,收集再進(jìn)一步加工生產(chǎn)氟苯。 每五分鐘收集反應(yīng)混合物的樣品。 所獲得的樣品,氟化重氮苯濃度在2.59摩爾/升到2.61 摩爾/升之間,基于注入亞硝基氟計(jì)算,相當(dāng)于苯胺生成氟化重氮苯轉(zhuǎn)化率的98%到100%之間。 |

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