Method for recovering and treating waste liquid generated during 4-cyano benzyl chloride production
A recovery treatment and waste liquid recovery technology, which is applied in chemical instruments and methods, preparation of organic compounds, purification/separation of carboxylic acid nitriles, etc., can solve problems such as environmental pollution and occupying a large space, so as to reduce production costs and prevent pollution , the effect of cheap raw materials
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Embodiment 1
[0026] Add 100g of industrial waste liquid, 3g of zinc chloride and 600g of water into a 1000mL four-necked flask equipped with a thermometer, a condenser and an electromagnetic stirrer at the same time. After heating and reflux for 8 hours of hydrolysis reaction, cool to room temperature and separate layers, take the upper layer of water and solid The mixture was filtered to obtain 20 g of p-cyanobenzaldehyde white product with a purity of 95.5%.
[0027] Take 50 g of the solid oil in the lower layer, add 120 g of 20% glacial acetic acid aqueous solution and 15 g of urotropine, heat and reflux for 3 hours, add hydrochloric acid to adjust the pH of the solution to about 3, continue the reaction for 3 hours, cool to 80 ° C, and then add NaOH aqueous solution to make The pH of the solution was about 6, cooled to room temperature, and filtered to obtain 10 g of a yellow crude product with a purity of 88%.
[0028] A total of 30 g of the above-mentioned crude product was added, 15...
Embodiment 2
[0030] The operation method is basically the same as in Example 1, the only difference is that 100g of industrial waste liquid, 6g of zinc chloride and 500g of water are added to a 1000mL four-neck flask at the same time, and after 16 hours of reflux hydrolysis reaction, it is cooled to room temperature and separated, and the upper layer of water-solid mixture is taken Filter to obtain 27g p-cyanobenzaldehyde crude product, purity 95%.
[0031] Take 50 g of the solid oil in the lower layer, add 150 g of 25% glacial acetic acid aqueous solution and 20 g of urotropine, reflux for 3 h, add hydrochloric acid to adjust the pH of the solution to about 2, continue the reaction for 2 h, cool to 80 ° C, then add NaOH to make the solution The pH was about 6, continued cooling to room temperature, and filtered 16g of crude product with a purity of 88.9%.
[0032] Add 172g of 20% ethanol aqueous solution to 43g of the above-mentioned crude product, heat to reflux, cool and crystallize, fi...
Embodiment 3
[0034] The operation method is basically the same as in Example 1, the only difference is that 100g of industrial waste liquid, 5g of zinc chloride and 650g of water are added to a 1000mL four-neck flask at the same time, and after 18 hours of reflux hydrolysis reaction, it is cooled to room temperature and separated, and the upper layer of water-solid mixture is taken Filter to obtain 34g p-cyanobenzaldehyde product, the purity is 96.6%.
[0035] Take 50 g of solid oil in the lower layer, add 150 g of 30% glacial acetic acid aqueous solution and 25 g of urotropine, reflux for 3 h, add hydrochloric acid to adjust the pH of the solution to about 1, continue the reaction for 1 h, cool to 80 ° C, then add NaOH to make the solution The pH was about 7, continued to cool to room temperature, and the filtered 15g crude product had a purity of 90.6%.
[0036] Add 200g of 20% methanol aqueous solution to 49g of the above-mentioned crude product, heat to reflux, cool and crystallize, fi...
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