Stable polyamide(s) prodn. using acid catalysts - comprises adding alumino silicate to deactivate the phosphorus contg. catalyst, preventing molecular wt. changes, hydrolysis and side reactions

摘要

Process uses acid catalysts of formula (R1O)(R2O)(R30)PO (IIA), H(R1O)(R2O)PO (IIB) or (R1O)R2O)(R3O)P (IIC) or their oligomers or polymers, in amts. such that the polyamide or reaction mixt. contains 10-200 (pref. 15-100, esp. pref. 20-80) ppm P (with R1-R3 = H, 1-25C (ar)alkyl, 6-25C (alk)aryl, Na, K or NH4). Aluminosilicates (III) are added as deactivators in amts. such that (II) are deactivated except for the case when (III) is added to the polycondensation starting mixt.. Pref. (II) are H3PO4, H3PO3, esters such as e.g. di-n-butyl, di-n-stearyl, diphenyl, triethyl, tristearyl, NaH2PO4, NH4H2PO4, H4P2O7, etc. Graham, Madrell or Kurrol salts, etc.. (III) are zeolites of formula M2/nO.Al2O3.xSiO2.yH2O (with M = metal gp. of Ia-VIIIa or Ib-IVb, pref. Ia, IIa, IIb, III, IVa or IVb, esp. Na, K, Ca, Mg or Zn; n = valency of M; x = 1-50, pref. 2-25, y = 0-9) or Al oxides of the kaolin, serpentine, montmorillonite or bentonite type. Amt. of (III) is such that wt. ratio P:(III) = 1:(6700-670,000), pref. 1:(33,000-330,000). The process is pref. used for the prodn. of PA 6, 6/6, 6T6, 6T/6, 6IT, 46, 610, 69, 612, 11, 12, 1212, or 6/66 or 6/12 copolyamide, pref. PA 6, 66 or copolyamides thereof, esp. pref. PA 6 or copolyamides based on PA 6. USE/ADVANTAGE - (III) are useful for deactivating phosphorus catalysts in (I) (claimed). Also claimed is the use of deactivated (I) for producing moulded prods., film, opt. reinforced fibres, semi-finished prods., composites, and finished prods. therefrom; these prods. are also claimed as such. Addn. of (III) deactivates residual (II) which can otherwise cause changes in molecular wt., hydrolysis or undesirable reactions during further processing.