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Titanium haude-organometal-organq- metal iodide catalyst for produc- tion of cis i,x-polybutadiene

Assignee: —
•
Filing: 1961-11-20
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Granted: 1965-03-09
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Expires: 1981-11-20
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Abstract

Abstract Isobutyl aluminium sesquiiodide is made by heating aluminium powder with isobutyl iodide, in toluene, and subsequently adding triisobutyl aluminium.ALSO:Polymers of butadiene-1, 3 of high cis 1, 4-content are made by effecting the polymerization in the presence of a catalyst system consisting of (1) a compound of the formula RnM where R is a hydrocarbon group containing up to 20 carbon atoms, M is Mg or Al, and n is an integer equal to the valency of M, (2) TiCl4 or TiBr4, and (3), an organometal iodide of the formula RxMyI2 where R is as under (1), M1 is Zn, Cd, Hg, Al, Ga, In, or Tl, I is iodine, X and Z are 1, 2, or 3, and Y is 1 or 2, and when Y=1, X+Z= the valence of metal M1, and when Y=2, X+Z =twice the valence of metal M1. The Specification contains an extensive list of catalysts and catalyst components. Exemplified catalysts are (1) isobutylaluminium sesquiiodide, triisobutyl aluminium, TiCl4, (2) di-n-butyl aluminium iodide, triethylaluminium, TiBr4, (3) di-n-propylaluminium iodide, triphenyl aluminium, TiCl4, (4) di-n-butylmagnesium, ethylaluminium sesquiiodide, TiCl4, and (5) diethyl magnesium, diisobutylaluminium iodide and TiBr4. The polymerization is effected by well-known "low-pressure" techniques.

Inventors

No inventors recorded.

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 13:10
CPC Classifications
C; C08; C08F; C08F136/00; C08F136/02; C08F136/04; C08F136/06

Claims Analysis

Total Claims: 2
Claim 1
Independent Claim 269 words
A PROCESS FOR PREPARING A RUBBERY POLYBUTADIENE CONTAINING IN THE RANGE OF 85 TO 98 PERCENT CIS 1,4-ADDITION WHICH COMPRISES CONTACTING 1,3-BUTADIENE WITH A CATALYST SYSTEM WHICH FORMS ON MIXING (1) AN ORGANOMETAL HAVING THE FORMULA RNM WHEREIN R IS SELECTED FROM THE GROUP CONSISTING OF ALKYL, CYCLOALKYL, ARYL, CYCLOALKYLALKYL, ARALKYL, ALKYLCYCLOALKYL, ARYLCYCLOALKYL, ALKARYL AND CYCLOALKYLARYL RADICALS, EACH R GROUP CONTAIING UP TO AND INCLUDING 20 CARBON ATOMS, M IS A METAL SELECTED FROM THE GROUP CONSISTING OF MAGNESIUM AND ALUMINUM AND N IS AN INTEGER EQUAL TO THE VALENCE OF METAL, M, (2) A TITANIUM TETRAHALIDE SELECTED FROM THE GROUP CONSISTING OF TITANIUM TETRACHLORIDE AND TITANIUM TETRABROMIDE, AND (3) AN ORGANOMETAL IODIDE OF THE FORMULA RXM''YIZ WHEREIN R IS AN ORGANIC RADICAL AS HEREINBEFORE DEFINED, M'' IS A METAL SELECTED FROM THE GROUP CONSISTING OF ZINC, CADMIUM, MERCURY, ALUMINUM, GALLIUM, INDIUM, AND THALLIUM, I IS IODINE, X AND Z ARE INTEGERS FROM 1 TO 3 AND Y IS AN INTEGER FROM 1 TO 2 AND WHEN Y=1, X+Z=THE VALENCE OF METAL M'' AND WHEN Y=2, X+Z=TWICE THE VALENCE OF METAL M'', THE MOLE RATIO OF THE RNMG COMPOUND TO SAID TITANIUM TETRAHALIDE BEING IN THE RANGE OF 1.05:1 TO 2:1, THE MOLE RATIO OF THE RNAL COMPOUND TO SAID TITANIUM TETRAHALIDE BEING IN THE RANGE OF 2:1 TO 20:1, THE MOLE RATIO OF SAID TITANIUM TETRAHALIDE TO SAID ORGANOMETAL IODIDE COMPOUND BEING IN THE RANGE OF 0.05:1 TO 0.7:1, SAID CONTACTING OCCURRING IN THE PRESENCE OF A HYDROCARBON DILUENT AT A TEMPERATURE RANGE OF -100 TO 250*C. AND UNDER AUTOGENOUS PRESSURE; AND RECOVERING THE RUBBERY CIS-POLYBUTADIENE SO PRODUCED.
Claim 2
Dependent Claim 269 words
A PROCESS FOR PREPARING A RUBBERY POLYBUTADIENE CONTAINING IN THE RANGE OF 85 TO 98 PERCENT CIS 1,4-ADDITION WHICH COMPRISES CONTACTING 1,3-BUTADIENE WITH A CATALYST SYSTEM WHICH FORMS ON MIXING (1) AN ORGANOMETAL HAVING THE FORMULA RNM WHEREIN R IS SELECTED FROM THE GROUP CONSISTING OF ALKYL, CYCLOALKYL, ARYL, CYCLOALKYLALKYL, ARALKYL, ALKYLCYCLOALKYL, ARYLCYCLOALKYL, ALKARYL AND CYCLOALKYLARYL RADICALS, EACH R GROUP CONTAIING UP TO AND INCLUDING 20 CARBON ATOMS, M IS A METAL SELECTED FROM THE GROUP CONSISTING OF MAGNESIUM AND ALUMINUM AND N IS AN INTEGER EQUAL TO THE VALENCE OF METAL, M, (2) A TITANIUM TETRAHALIDE SELECTED FROM THE GROUP CONSISTING OF TITANIUM TETRACHLORIDE AND TITANIUM TETRABROMIDE, AND (3) AN ORGANOMETAL IODIDE OF THE FORMULA RXM''YIZ WHEREIN R IS AN ORGANIC RADICAL AS HEREINBEFORE DEFINED, M'' IS A METAL SELECTED FROM THE GROUP CONSISTING OF ZINC, CADMIUM, MERCURY, ALUMINUM, GALLIUM, INDIUM, AND THALLIUM, I IS IODINE, X AND Z ARE INTEGERS FROM 1 TO 3 AND Y IS AN INTEGER FROM 1 TO 2 AND WHEN Y=1, X+Z=THE VALENCE OF METAL M'' AND WHEN Y=2, X+Z=TWICE THE VALENCE OF METAL M'', THE MOLE RATIO OF THE RNMG COMPOUND TO SAID TITANIUM TETRAHALIDE BEING IN THE RANGE OF 1.05:1 TO 2:1, THE MOLE RATIO OF THE RNAL COMPOUND TO SAID TITANIUM TETRAHALIDE BEING IN THE RANGE OF 2:1 TO 20:1, THE MOLE RATIO OF SAID TITANIUM TETRAHALIDE TO SAID ORGANOMETAL IODIDE COMPOUND BEING IN THE RANGE OF 0.05:1 TO 0.7:1, SAID CONTACTING OCCURRING IN THE PRESENCE OF A HYDROCARBON DILUENT AT A TEMPERATURE RANGE OF -100 TO 250*C. AND UNDER AUTOGENOUS PRESSURE; AND RECOVERING THE RUBBERY CIS-POLYBUTADIENE SO PRODUCED.

References Cited (Backward Citations)

US2976271A Cited
US3095406A Cited
FR1256231A Cited
BE591994A Cited
DE1113311B Cited
US3076795A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1968-03-08 1968-09-07 1969-03-09 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1972-03-08 1972-09-07 1973-03-09 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1976-03-08 1976-09-07 1977-03-09 $7700.00 Window Closed / Lapsed

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