Beta crystalline modification of 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tert-buytl-1,1'-biphenyl- 2,2'-diyl)phosphite]
AssigneeCiba-Geigy Corporation
InventorsStephen D. Pastor, Sai P. Shum
Life of this patent
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Abstract
The beta crystalline modification of 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tertbutyl-1,1'-biphenyl-2,2 '-diyl) phosphite] is obtained by crystallizing said compound from the melt at elevated temperatures. The beta crystalline form is an effective process stabilizer for polyolefins, particularly polypropylene.
Claims8
A process for the preparation of the beta, triclinic crystalline form of the compound 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2, 2'-diyl)phosphite], characterized by melting in the range of 200.degree.-207.degree. C. and by an X-ray diffraction pattern exhibiting lines of very high intensity at 8.4 and 17;
- lines of high intensity at 9.9, 10.6, 11.4, 17.5, 19.1, 20.2;
- lines of medium intensity at 4.6, 4.9, 7.1, 12.7, 13.2, 13.6, 15.3, 15.8, 16.4, 16.7, 18.4, 19.7, 21.7, 23.4;
- and lines of weak intensity at 7.8, 8.8, 9.4, 12, 14.1, 14.6, 21, 22.3, 22.8, 23.9, 24.7, 25.3, 25.5, 26.4, 27.27.7, 28.4 and a relative absolute configuration of the three stereo axes of the dibenzo[d,f][1,3,2]dioxaphosphepin rings of R*,R*,S*, which comprises
- heating a melt of the compound 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2, 2'-diyl)phosphite] at a temperature in the range of 170.degree. to 200.degree. C. to crystallize the novel beta crystalline modification.
A process for the preparation of the beta, triclinic crystalline form of the compound 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2, 2'-diyl)phosphite], characterized by melting in the range of 200.degree.-207.degree. C. and by an X-ray diffraction pattern exhibiting lines of very high intensity at 8.4 and 17;
- lines of high intensity at 9.9, 10.6, 11.4, 17.5, 19.1, 20.2;
- lines of medium intensity at 4.6, 4.9, 7.1, 12.7, 13.2, 13.6, 15.3, 15.8, 16.4, 16.7, 18.4, 19.7, 21.7, 23.4;
- and lines of weak intensity at 7.8, 8.8, 9.4, 12, 14.1, 14.6, 21, 22.3, 22.8, 23.9, 24.7, 25.3, 25.5, 26.4, 27.27.7, 28.4 and a relative absolute configuration of the three stereo axes of the dibenzo[d,f][1,3,2]dioxaphosphepin rings of R*,R*,S*, which comprises
- crystallizing or recrystallizing said compound from a mixture of an aromatic hydrocarbon solvent and an alcohol of 4 to 8 carbon atoms;
- from a mixture of an aliphatic ketone and an alcohol;
- or from a mixture of an aromatic hydrocarbon solvent and an aliphatic ketone.
The beta, triclinic crystalline form of 2,2',2"-nitrilo[triethyl-tris-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2, 2'-diyl)phosphite], characterized by melting in the range of 200.degree.-207.degree. C. and by an X-ray diffraction pattern exhibiting lines of very high intensity at 8.4 and 17;
- lines of high intensity at 9.9, 10.6, 11.4, 17.5, 19.1, 20.2;
- lines of medium intensity at 4.6, 4.9, 7.1, 12.7, 13.2, 13.6, 15.3, 15.8, 16.4, 16.7, 18.4, 19.7, 21.7, 23.4;
- and lines of weak intensity at 7.8, 8.8, 9.4, 12, 14.1, 14.6, 21, 22.3, 22.8, 23.9, 24.7, 25.3, 25.5, 26.4, 27.27.7, 28.4 and a relative absolute configuration of the three stereo axes of the dibenzo[d,f][1,3,2]dioxaphosphepin rings of R*,R*,S*.
Dependencies are inferred from the claim text.