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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.

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sltmac(½ð±Ò+3): ¸ÐлӦÖú~~ 2011-07-31 15:20:14
sltmac(½ð±Ò+10): 2011-08-05 08:25:52
EXAMPLE 4
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Diazotization of Aniline in a Cross-Flow Recycle Reactor
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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.
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sltmac(½ð±Ò+10): 2011-08-05 08:25:59
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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.
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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.
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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.
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The nitrosyl fluoride-HF solution was injected incrementally into lines 38, 44 and 48 immediately prior to each of the three static mixers.
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The proportions of nitrosyl fluoride fed to static mixer 58, 74 and 68 respectively, were 50%, 40% and 10%.
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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. °ÑÑÇÏõ»ù·úÈÜÒºÓÃһСʱÔÚ10¡æÁ¬ÐøÊäËÍ£¬Í¨¹ýÃÜ·â¹Þ36ÖУ¬ÇÒÁ÷ËÙ¿ØÖÆÔÚ209ºÁÉý/·ÖÖÓ£¬ÊÇͨ¹ý¿ØÖÆ·§£¨Î´ÏÔʾ£©£¬Ê¹´óÔ¼7£¥µÄ±½°·½øÁÏÊä³ö(δת»¯µÄ)70¡£
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