Photosensitive adsorption of water vapour on wool. Part II

✍ Scribed by Bright, N. F. H. ;Carson, T.

• Publisher: Wiley (John Wiley & Sons)
• Year: 1948
• Weight: 240 KB
• Volume: 67
• Category: Article
• ISSN: 0368-4075
• DOI: 10.1002/jctb.5000671210

✦ Synopsis

An attempt was made to redistil the water layer in order to recover small amounts of acrylonitrile, but some volatile material present solidified in the condenser causing a blockage, and owing to the development of pressure the bulk had to be ^ettisoned The water-white crude acrylonitrile was dried by treating three times with calcium chloride (total 7 lb.), to give 66.5 Ib. of dry product. This material was redistilled in the same unit (without using the reflux condenser as such) collecting the material in the range 78-82' to give 54 Ib. product (= 59.0% theory), and leaving 8 Ib. 6 oz. of a thick brown oily residue in the vessel. There was a loss of 4 lb. 2 02. on this distillation but pressure testing failed to detect any leaks in the plant. Small quantities of the thick oily residue were distilled from an oil heated 2 1. flask in order to obtain any acrylonitrile not removed. After a quantity ofa thin white liquid having a strong ammoniacal odour distilled over, the residue in the flask suddenly frothed vigorously and set to a brown hard mass.

The distilled material had the analysis : N = 24'9% 94*5y0

C3H3N ; H20 = 0.88%~ but it is not known how reliable the nitrogen analysis is for this substance.

The distilled acrylonitrile was stabilized by the addition of 0.1% by weight of hydroquinone before being charged into tin . lined drums for transit.

Acknowledgements

The heat of reaction of ethylene chlorhydrin and sodium cyanide was determined by Mr. M. J. Thornton and part of the experimental work on the dehydration of ethylene cyanhydrin to acrylonitrile was carried out with the assistance of Mr. K. S.