Ammonia → 1,4-Benzenedimethanamine

温度

120 °C

A stirred autoclave was charged with 400 ml. tetrahydrofuran (THF), 100 ml. ammonia, 50 g. terephthalonitrile (TPN) and 6.0 g. cobalt supported catalyst and various amounts of water. The autoclave was heated to 120° C. Hydrogen was introduced rapidly until the selected pressure was reached. The absorption of hydrogen started immediately and additional hydrogen was added to keep the pressure at the selected level. The course of the reaction was monitored by measuring the volume of hydrogen consumed and by periodic withdrawal of a small sample of the reaction mixture for analysis. When the analysis indicated that all of the terephthalonitrile had reacted, the agitation was stopped and the reactor was cooled rapidly and vented. The reaction mixture was filtered to recover the catalyst and then was flash evaporated to remove solvent. The residual oil was flash distilled at about 100° C. and 0.5 mm Hg. to give practically pure p-xylylene diamine. A small amount of high boiling residue remained in the distillation pot. Results of experiments conducted with various amounts of water and at 1500 and 2500 psig are listed in Table I.

1. additionA stirred autoclave was charged with 400 ml
2. customThe absorption of hydrogen
3. additionadditional hydrogen was added
4. customconsumed and by periodic withdrawal of a small sample of the reaction mixture for analysis
5. customhad reacted
6. temperaturethe reactor was cooled rapidly
7. filtrationThe reaction mixture was filtered
8. customto recover the catalyst
9. customevaporated
10. customto remove solvent
11. distillationdistilled at about 100° C.

ORDレコード

ord-7e6cd9f6c5f9464fbaee0cb1ba972c3b

出典データセット

uspto-grants-1980_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04222961