Reference

Polymerization of a-olefin using a specified deactivator for catalyst

Polymerization of a-olefin using a specified deactivator for catalyst. (Asahi Chemical Industry Co., Ltd., Japan). Jpn. Kokai Tokkyo Koho JP 59071311 A2 23 Apr 1984 Showa, 12 pp. (Japanese). (Japan). CODEN: JKXXAF. CLASS: IC: C08F010-02; C08F006-12. APPLICATION: JP 82-180016 15 Oct 1982. DOCUMENT TYPE: Patent CA Section: 35 (Chemistry of Synthetic High Polymers) After the polymn. of ethylene optionally with a C3-18 a-olefin at 3130° by a Ziegler-type catalyst contg. Ti and Mg in the presence or absence of a solvent an alkali or alkali earth alkoxide is added as a deactivator in the form of a hydrocarbon suspension, solid, or melt, the monomer and/or inert solvent is sepd., and the deactivator or polymer contg. it is removed. As a hydrocarbon-sol. org. Mg compd. MaMgbRp1Rq2Xr1Xs2 [M = Al, Zn, B, Be or Li; b 3 1, p, q, r, and s 3 0; p+q+r+s = ma + 2b, 0 ￡ (r + s)/(a + b) ￡ 1.0; m = valence of M; R1 and R2 = C1-20 hydrocarbyl, X1 and X2 = H, OR3, OSiR4R5R6, NR7R8 or SR9 (R3, R7, R8 and R9 = C1-20 hydrocarboyl, and R4, R5, and R6 = H or C1-20 hydrocarbyl)] is used, with a Ti(OR10)n.X4-n (R10 = C1-20 hydrocarbyl; X = halogen; 0 ￡ n ￡ 3) at mol ratio 1:1.1-4.0 to make a Ti component. For example, to a mixt. of 1.6 L 0.5 M HSiCl3 [10025-78-2] hexane soln. and 1.2 L hexane at 70° were added 0.45 L Al0.15MgBu1.75 (metal concn. 0.9 M) octane soln. and 0.35 L hexane at 70° in 1 h, and the mixt. was treated with 0.7 g TiCl4 in 0.6 L hexane at 70° for 1 h to give a solid component. To a 100 L autoclave were continuously supplied 1.0 g/h above solid, 200 L/h 0.1 mM AlEt3 [97-93-8] cyclohexane soln., 25 kg/h ethylene, and 1 kg/h H2, and polymn. was carried out at 200° and 80 kg/cm2 to give 20 kg/h polyethylene [9002-88-4] at conversion 80%. The deactivator (NaOEt [141-52-6]; 2% in hexane) was supplied at 40 mmol/L to the outgoing polymer from the reactor, the mixt. heated to 250° and the pressure reduced to 1 kg/cm2, and the product fed to the separator to give a polymer slurry from the bottom.

Polymerization of a-olefin using a specified deactivator for a catalyst

Polymerization of a-olefin using a specified deactivator for a catalyst. (Asahi Chemical Industry Co., Ltd., Japan). Jpn. Kokai Tokkyo Koho JP 59071310 A2 23 Apr 1984 Showa, 12 pp. (Japanese). (Japan). CODEN: JKXXAF. CLASS: IC: C08F010-02; C08F006-12. APPLICATION: JP 82-180015 15 Oct 1982. DOCUMENT TYPE: Patent CA Section: 35 (Chemistry of Synthetic High Polymers) After the polymn. of ethylene optionally with a C3-18 a-olefin at 3130° by a Ziegler-type catalyst contg. Mg and Ti in the presence or absence of a solvent, an alkali or alk. earth aluminate is added as a deactivator in the form of hydrocarbon suspension, a solid or a melt, the monomer and/or inert solvent is sepd., and the deactivator or polymer contg. it is removed. As a hydrocarbon-sol. org. Mg compd. a MaMgbRp1Rq2Xr1Xs2 [M = Al, Zn, B, Be or Li; b 3 1, a, p, q, r, and s 30; p+q+r+s = ma + 2b, 0 ￡ (r + s)/(a + b) ￡ 1.0; m = valence of M; R1 and R2 = C1-20 hydrocarbyl, X1 and X2 = H, OR3, OSiR4R5R6, NR7R8 or SR9 (R3, R7, R8 and R9 = C1-20 hydrocarbyl, and R4, R5, and R6 = H or C1-20 hydrocarbyl)] is used, with Ti(OR10)n.X4-n (R10 = C1-20 hydrocarbyl; X = halogen; 0 ￡ n ￡ 3) at mol ratio 1:1.1-4.0 to give a catalyst component which then combined with an organoaluminum compd. For example, to a mixt. of 1.6 L 0.5 M HSiCl3 [10025-78-2] hexane soln. and 1.2 L hexane at 70° were added 0.45 L Al0.15MgBu1.75 (metal concn. 0.9 M) octane soln. and 0.35 L hexane at 70° in 1 h and the mixt. was treated with 0.7 g TiCl4 in 0.6 L hexane at 70° for 1 h to give a solid component. To a 100 L autoclave were continuously supplied 1.0 g/h above solid, 200 L/h 0.1 mM AlEt3 cyclohexane soln., 25 kg/h ethylene, and 1 kg/h H2, and polymn. was carried out at 200° and 80 kg/cm2 to give 20 kg/h polyethylene [9002-88-4] at conversion 80%. The deactivator (Na aluminate; 2% slurry in hexane) was supplied at 40 mmol/L to the outgoing polymer slurry from the bottom of the reactor, the mixt. heated to 250° and the pressure reduced to 1 kg/cm2, the mixt. introduced to the separator, and the polymer slurry drawn from the bottom.