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xuh2so4

铁杆木虫 (正式写手)

[交流] 【求助】电解不能发生原因分析已有5人参与


该反应文献是用银做阴极,含镍不锈钢做阳极,-1.3V电解。发现没产物出现。我用的银网做电极,不锈钢板做阳极。求高人分析分析。
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xuh2so4

铁杆木虫 (正式写手)

引用回帖:
Originally posted by rain27 at 2010-06-01 16:00:40:
可能是你电解电位的问题吧。你用恒电位还是恒电流电解的?-1.3V电解是相对于Ag/AgCl嘛?

是用恒电位,就是阴极与参比电极之间的电压是1.3V
5楼2010-06-01 20:08:50
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小桥.流水.猪

木虫 (知名作家)

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xuh2so4(金币+1):谢谢参与
电解一般要含有羟基,羧基类似的官能团,这个东西,恐怕很难
永恒的只有信念。
2楼2010-06-01 14:43:22
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xuh2so4

铁杆木虫 (正式写手)

引用回帖:
Originally posted by 小桥.流水.猪 at 2010-06-01 14:43:22:
电解一般要含有羟基,羧基类似的官能团,这个东西,恐怕很难

文献都做到公斤级了,不可能是反应本身的问题文献描述是

4-amino-3,6dichloropyridine-2-carboxylic acid (batch cell)
The cell was a 180 mL beaker (2 in. (5.1 cm) diameter x 4.5 in. (11.4 cm) tall). The silver mesh cathode consisted of a 1 in. (2.5 cm) x 4 in. (10.2 cm) strip placed around the inside wall of the beaker approximately 0.5 in. (1.3 cm) off the bottom and had a 0.5 in. (1.3 cm) wide strip extending out the top of the beaker to which the power supply was attached.

The anode was a 0.75 in. (1.9 cm) diameter x 6 in.

(15.2 cm) long graphite rod that was supported by a rubber stopper in the middle of the beaker and extended to about 0.5 in. (1.3 cm) off the bottom.

The working potential of the cathode was controlled relative to an Ag/AgCl (3.0 M Cl-) reference electrode positioned between the silver mesh and the wall of the beaker.

The silver mesh cathode was activated by anodization at +0.7 volt (v) in a 2% sodium hydroxide and 1% sodium chloride solution in water followed by reverse polarization. After activation, the solution was replaced with a solution of 81 mL of water, 5.1 g (0.0213 moles) of 4-amino-3,5,6-trichloropicolinic acid, and 2.8 g (0.0426 moles) of 85% KOH. After sparging with a slow stream of nitrogen, the electrolysis was carried out at a working potential of -1.3 to-1.35 volts for 2 hours at ambient temperature. The current started at 0.83 amps and gradually decreased to 0.25 amps after the two hours.

A total of 5000 coulombs were passed through the solution (theory for reduction of one chlorine off the pyridine ring is 2050 coulombs). Analysis of the crude product solution by gradient elution HPLC showed the disappearance of the starting material and the appearance of a single peak later identified as 4amino-3,6-dichloropicolinic acid

大家看看我反应有问题吗? 以前没做过电化学,汗
3楼2010-06-01 15:07:36
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rain27

木虫 (小有名气)


xuh2so4(金币+1):谢谢参与
可能是你电解电位的问题吧。你用恒电位还是恒电流电解的?-1.3V电解是相对于Ag/AgCl嘛?
4楼2010-06-01 16:00:40
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