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Process for hydrogenation of diene (CO) polymers

A composition and compound technology, applied in chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, chemical/physical processes, etc., can solve complex methods, unsatisfactory hydrogenation rates, large amounts of titanium And other issues

Inactive Publication Date: 2004-05-05
ENICHEM SPA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The method of EP-A-601,953 is also complicated because it contains 2 TiCl 2 Preparation and Isolation of Special Titanium Dicyclopentadienyl Derivatives
[0015] The catalysts in any case of the prior art have the disadvantages of requiring a large amount of titanium and an unsatisfactory rate of hydrogenation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1A) Preparation of catalytic composition

[0063] 20ml cyclohexane, 1.8ml Cp 2 TiCl 2 THF solution with a concentration of 10.36g / l (equal to 0.019g = 0.075mmol), 0.7ml consists of 10% dibutylmagnesium (equal to 51.94g = 0.375mmol), where Mg / Ti = 5, and 1% triethylaluminum (equivalent to 5.19mg=0.045mmol), where Al / Ti=0.6 composition of n-heptane (d=0.730g / ml) solution, under argon atmosphere, the above components were added in order to a 100ml Schlenk tube.

[0064] 1B.1) hydrogenation reaction

[0065]600 g of a polymer solution of 7.5 wt% SBS in cyclohexane (45% vinyl, percent styrene / butadiene 33 / 67, Mw 170000) was transferred to a 1 liter Buchi type steel reactor; The mixture was stirred at 1000 rpm, fed with hydrogen up to 6 bar, and the temperature was thermostatted at 100°C. The catalytic composition according to part 1A was charged to the reactor together with an amount of titanium of 80 ppm relative to the dry polymer, the olefinic double bond / titanium...

Embodiment 2

[0069] 2A) Preparation of catalytic composition

[0070] 20ml cyclohexane, 1.36ml Cp 2 TiCl 2 Concentration is 10.36g / l (equivalent to 0.014g=0.056mmol) THF solution, 0.7ml n-heptane (d=0.730g / ml) solution, by 10% dibutylmagnesium (38.94g=0.281mmol), wherein Mg / Ti molar ratio = 5, and 1% triethylaluminum (3.89mg = 0.034mmol), wherein Al / Ti molar ratio = 0.6 composition, under argon atmosphere, the above components were added to a 100ml Schlenk tube in sequence middle. The mixture was then stirred at room temperature under an argon atmosphere for 20 minutes.

[0071] 2B.1) hydrogenation reaction

[0072] 600 g of a polymer solution of 7.5 wt% SBS in cyclohexane (45% vinyl, percent styrene / butadiene 33 / 67, Mw 170000) was transferred to a 1 liter Buchi type steel reactor; The mixture was stirred at 1000 rpm, fed with hydrogen up to 6 bar, and the temperature was thermostatted at 100°C. The catalytic composition according to part 2A was introduced into the reactor togeth...

Embodiment 3

[0077] 3A) Preparation of catalytic composition

[0078] 20ml cyclohexane, 0.87ml Cp 2 TiCl 2 Concentration is 10.36g / l (equivalent to 0.009g=0.0375mmol) THF solution, 0.35ml n-heptane (d=0.730g / ml) solution, by 10% dibutylmagnesium (25.9mg=0.187mmol), wherein Mg / Ti=5, and 1% triethylaluminum (2.59mg=0.023mmol), wherein Al / Ti=0.6 composition, under argon atmosphere, the above components were sequentially added to a 100ml Schlenk tube. The mixture was then stirred at room temperature under an argon atmosphere for 20 minutes.

[0079] 3B.1) hydrogenation reaction

[0080] 600 g of a polymer solution of 7.5 wt% SBS in cyclohexane (45% vinyl, styrene / butadiene percentage composition 33 / 67, Mw 170000) was transferred to a 1 liter Buchi type steel reactor; The mixture was stirred at 1000 rpm, fed with hydrogen up to 6 bar, and the temperature was thermostatted at 100°C. The catalytic composition according to part 3A was fed into the reactor together with an amount of titani...

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PUM

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Abstract

Catalytic composition effective in the hydrogenation of olefinic double bonds prepared by reaction between:(A) at least one cyclopentadienyl complex of a transition metal having general formula (I) (R)(R1)M1(R2)(R3) wherein R is an anion containing an eta5-cyclopentadienyl ring coordinated to M1; M1 is selected from titanium, zirconium and hafnium; R2 and R3, the same or different, are organic or inorganic anion groups bound to M1; R1 is selected from cyclopentadienyl and R2;(B) an alkylating composition essentially consisting of:(b1) an organometallic compound having general formula (II) M2 (R4)(R5), wherein M2 is selected from Zn and Mg;(b2) an organoderivative of aluminum having general formula (III) Al(R6)3.

Description

technical field [0001] The present invention relates to a catalytic composition which can be used for the hydrogenation of ethylenically unsaturated compounds, in particular to a catalytic composition for the selective hydrogenation of conjugated diene polymers and copolymers. Background technique [0002] Polymers obtained by (co)polymerization of conjugated dienes are widely used commercially. [0003] On the polymer chain these (co)polymers have ethylenic double bonds for vulcanization, which have poor stability, especially poor oxidation resistance. [0004] In particular, block copolymers obtained from conjugated dienes and vinyl-substituted arenes are used in a non-vulcanized manner as thermoplastic elastomers or as impact-resistant transparent resins or as modifiers for styrenic or olefinic resins. Due to the presence of unsaturated double bonds in the polymer chain, the above block copolymers have poor oxidation resistance, ozone resistance, a...

Claims

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Application Information

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IPC IPC(8): B01J31/12B01J31/14B01J31/22C08C19/02C08F8/04C08F297/04
CPCB01J2531/49B01J2231/645C08F8/04B01J31/143B01J31/2295B01J31/128C08C19/02B01J2531/48B01J31/122B01J2531/46
Inventor G·T·维奥拉A·瓦利里C·卡瓦洛
Owner ENICHEM SPA
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