US3928303A — Process for producing butadiene polymer

Claim 1

Independent Claim 121 words

A PROCESS FOR THE POLYMERIZATION OF BUTADIENE TO GIVE A RUBBER-LIKE SOLID WHICH COMPRISES CONTACTING BUTADIENE WITH A CATALYST SYSTMEM CONSISTING ESSENTIALLY OF (A) AN ORGANIC ALUMINUM FLUORIDE COMPOUND OF THE FORMULA: ALR3-NFN WHEREIN R IS ALKYL, ARYL OR ARALKYL AND N IS A REAL NUMBER LARGER THAN 1 AND SMALLER THAN 2 AND (B) AN ORGANIC NICKEL COMPOUND SELECTED FROM THE GROUP CONSISTING OF NICKEL SALTS OF ORGANIC CARBOXYLIC ACIDS, NICKEL SALTS OF ORGANIC COMPLEX COMPOUNDS, TETRACARBONYL NICKEL AND $-BONDED ORGANIC NICKEL COMPOUNDS, THE MOLAR RATIO OF THE ORGANIC ALUMINUM FLUORIDE COMPOUND TO THE ORGANIC NICKEL COMPOUND BEING IN A RANGE OF FROM 1:1 TO 1000:1, TO PRODUCE SAID RUBBER-LIKE SOLID BUTADIENE POLYMER HAVING A HIGH CONTENT OF CIS-1,4 STRUCTURE.

Claim 2

Dependent Claim 121 words

A PROCESS FOR THE POLYMERIZATION OF BUTADIENE TO GIVE A RUBBER-LIKE SOLID WHICH COMPRISES CONTACTING BUTADIENE WITH A CATALYST SYSTMEM CONSISTING ESSENTIALLY OF (A) AN ORGANIC ALUMINUM FLUORIDE COMPOUND OF THE FORMULA: ALR3-NFN WHEREIN R IS ALKYL, ARYL OR ARALKYL AND N IS A REAL NUMBER LARGER THAN 1 AND SMALLER THAN 2 AND (B) AN ORGANIC NICKEL COMPOUND SELECTED FROM THE GROUP CONSISTING OF NICKEL SALTS OF ORGANIC CARBOXYLIC ACIDS, NICKEL SALTS OF ORGANIC COMPLEX COMPOUNDS, TETRACARBONYL NICKEL AND $-BONDED ORGANIC NICKEL COMPOUNDS, THE MOLAR RATIO OF THE ORGANIC ALUMINUM FLUORIDE COMPOUND TO THE ORGANIC NICKEL COMPOUND BEING IN A RANGE OF FROM 1:1 TO 1000:1, TO PRODUCE SAID RUBBER-LIKE SOLID BUTADIENE POLYMER HAVING A HIGH CONTENT OF CIS-1,4 STRUCTURE.

Claim 3

Dependent Claim 12 words

The process according to claim 1, wherein n is 1.2 to 1.8.

Claim 4

Dependent Claim 29 words

The process according to claim 1, wherein the nickel compound is used in an amount of from 0.0005 to 2.0 mmol based on 1 mol of the butadiene monomer.

Claim 5

Dependent Claim 28 words

The process according to claim 1, wherein the molar ratio of the organic aluminum fluoride compound to the nickel compound is in a range from 1 to 100:1.

Claim 6

Dependent Claim 19 words

The process according to claim 1, wherein the polymerization is carried out at a temperature from -20* to 150*C.

Claim 7

Dependent Claim 16 words

The process according to claim 1, wherein the polymerization is carried out in a liquid medium.

Claim 8

Dependent Claim 17 words

The process according to claim 1, wherein the polymerization is carried out in the presence of water.

Claim 9

Dependent Claim 27 words

The process according to claim 7, wherein the amount of water is from 0.01 to (6-3n) mol based on 1 mol of the organic aluminum fluoride compound.

Claim 10

Dependent Claim 42 words

The process according to claim 1, wherein the polymerization is carried out in the presence of a molecular weight regulator selected from the group consisting of halogenated alcohols, halogenated carboxylic acids, halogenated carboxylic acid anhydrides, halogenated ketones, halogenated aldehydes, phenols and hydroquinones.

Claim 11

Dependent Claim 112 words

The process according to claim 9, wherein the molecular weight regulator is (1) a halogenated alcohol of the formula: RxOH wherein Rx is halogenated alkyl, (2) a halogenated carboxylic acid of the formula: RyCOOH wherein Ry is halogenated alkyl or halogenated aryl, (3) a halogenated carboxylic acid anhydride of the formula: (RyCO)2O wherein Ry is as defined above, (4) a halogenated ketone of the formula: Rz-CO-Rz'' wherein Rz and Rz'' are each alkyl, halogenated alkyl, aryl or halogenated aryl and at least one of them is always halogenated alkyl or halogenated aryl, (5) a halogenated aldehyde of the formula: Ry-CHO wherein Ry is as defined above, (6) a phenol of the formula:

Claim 12

Dependent Claim 30 words

The process according to claim 9, wherein the amount of the molecular weight regulator is from 0.01 to 50 mol based on 1 mol of the organic aluminum fluoride compound.

Claim 13

Dependent Claim 147 words

A process for the polymerization of butadiene to give a rubber-like solid which comprises contacting butadiene with a catalyst system consisting of (A) an organic aluminum fluoride compound of the formula: AlR3-nFn wherein R is alkyl, aryl or aralkyl and n is a real number larger than 1 and smaller than 2 and (B) an organic nickel compound selected from the group consisting of nickel acetate, nickel naphthenate, nickel octanoate, nickel benzoate, nickel chloride-pyridine complex, tris(dipyridyl) nickel chloride, bis(ethylenediamine)nickel sulfate, bis-acetylacetonate nickel, bis-ethylacetoacetate nickel, bis-dimethylglyoxymato nickel, tetracarbonyl nickel, bis( pi -allyl)nickel, bis( pi -methallyl)nickel, bis( pi -crotyl) nickel, bis( pi -cyclooctenyl)nickel and bis( pi -cyclopentenyl) nickel, the molar ratio of the organic aluminum fluoride compound to the organic nickel compound being in the range of from 1 : 1 to 1000 : 1, to produce said rubber-like solid butadiene polymer having a high content of cis-1,4 structure.

Claim 14

Dependent Claim 147 words

A process for the polymerization of butadiene to give a rubber-like solid which comprises contacting butadiene with a catalyst system consisting of (A) an organic aluminum fluoride compound of the formula: AlR3-nFn wherein R is alkyl, aryl or aralkyl and n is a real number larger than 1 and smaller than 2 and (B) an organic nickel compound selected from the group consisting of nickel acetate, nickel naphthenate, nickel octanoate, nickel benzoate, nickel chloride-pyridine complex, tris(dipyridyl) nickel chloride, bis(ethylenediamine)nickel sulfate, bis-acetylacetonate nickel, bis-ethylacetoacetate nickel, bis-dimethylglyoxymato nickel, tetracarbonyl nickel, bis( pi -allyl)nickel, bis( pi -methallyl)nickel, bis( pi -crotyl) nickel, bis( pi -cyclooctenyl)nickel and bis( pi -cyclopentenyl) nickel, the molar ratio of the organic aluminum fluoride compound to the organic nickel compound being in the range of from 1 : 1 to 1000 : 1, to produce said rubber-like solid butadiene polymer having a high content of cis-1,4 structure.

Claim 15

Dependent Claim 29 words

The process according to claim 12, wherein the nickel compound is used in an amount of from 0.0005 to 2.0 mmol based on 1 mol of the butadiene monomer.

Claim 16

Dependent Claim 20 words

The process according to claim 13, wherein the polymerization is carried out at a temperature of from -20* to 150*C.

Claim 17

Dependent Claim 33 words

the process according to claim 13, wherein the polymerization is carried out in the presence of from 0.01 to (6-3n) mol of water based on 1 mol of the organic aluminum fluoride compound.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1978-12-22	1979-06-23	1979-12-23	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1982-12-22	1983-06-23	1983-12-23	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1986-12-22	1987-06-23	1987-12-23	$7700.00	Window Closed / Lapsed

Process for producing butadiene polymer

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