US4151111A — Process for preparing titanium trichloride compos…

Claim 1

Independent Claim 128 words

A process for preparing a titanium trichloride composition comprising steps of: reducing titanium tetrachloride with an organoaluminum compound to produce a titanium trichloride composition having a β-crystal structure; then heat treating the resulting titanium trichloride composition having a β-crystal structure, and subsequently pulverizing the heat-treated titanium trichloride to produce a titanium trichloride composition in the δ form containing substantially no titanium trichloride having a β-crystal structure; then treating the pulverized titanium trichloride composition with an ether complexing agent for said titanium trichloride selected from the group consisting of diethyl ether, di-n-butyl ether, di-n-amyl ether, diisoamyl ether, di-n-hexyl ether, anisole, diphenyl ether, diethylene glycol dimethyl ether, and diethylene glycol mono-n-butyl ether; and treating said titanium trichloride composition which has been treated with said complexing agent with an interhalogen compound.

Claim 2

Dependent Claim 128 words

A process for preparing a titanium trichloride composition comprising steps of: reducing titanium tetrachloride with an organoaluminum compound to produce a titanium trichloride composition having a β-crystal structure; then heat treating the resulting titanium trichloride composition having a β-crystal structure, and subsequently pulverizing the heat-treated titanium trichloride to produce a titanium trichloride composition in the δ form containing substantially no titanium trichloride having a β-crystal structure; then treating the pulverized titanium trichloride composition with an ether complexing agent for said titanium trichloride selected from the group consisting of diethyl ether, di-n-butyl ether, di-n-amyl ether, diisoamyl ether, di-n-hexyl ether, anisole, diphenyl ether, diethylene glycol dimethyl ether, and diethylene glycol mono-n-butyl ether; and treating said titanium trichloride composition which has been treated with said complexing agent with an interhalogen compound.

Claim 3

Dependent Claim 43 words

The process as claimed in claim 1 in which the organoaluminum compound has the formula: Al R.sub.n Cl.sub.3-n wherein n is a number satisfying an equation: 0 < n ≦ 3 and R is a hydrocarbon residue having 1 to 10 carbon atoms.

Claim 4

Dependent Claim 28 words

The process as claimed in claim 2 in which the organoaluminum compound is a member selected from the group consisting of diethylaluminum chloride, ethylaluminum sesquichloride and ethylaluminum dichloride.

Claim 5

Dependent Claim 22 words

The process as claimed in claim 1 in which the reduction temperature is in the range of -30° C. to +30° C.

Claim 6

Dependent Claim 41 words

The process as claimed in claim 1 in which the titanium trichloride composition having a β- crystal structure is heat treated at a temperature of 100° to 200° C., under an atmosphere of an inert gas for 1 to 10 hours.

Claim 7

Dependent Claim 21 words

The process as claimed in claim 1 in which the heat treated titanium trichloride is pulverized for 10 to 72 hours.

Claim 8

Dependent Claim 36 words

The process as claimed in claim 1 in which the heat treated titanium trichloride is pulverized in the presence of titanium tetrachloride to produce titanium trichloride having substantially no titanium trichloride having a β- crystal structure.

Claim 9

Dependent Claim 28 words

The process as claimed in claim 7 in which the titanium tetrachloride is in a quantity of from 0.03 to 0.3 mole per mole of the titanium trichloride.

Claim 10

Dependent Claim 28 words

The process as claimed in claim 1 in which the complexing agent is in a quantity of from 0.3 to 3.0 moles per mole of the titanium trichloride.

Claim 11

Dependent Claim 31 words

The process as claimed in claim 1 in which the complexing is carried out at a temperature of from room temperature to 100° C. for from 30 minutes to 4 hours.

Claim 12

Dependent Claim 32 words

The process as claimed to claim 1 in which the interhalogen compound has the formula XY.sub.n wherein X and Y are different halogen atoms, and n is 1, 3, 5 or 7.

Claim 13

Dependent Claim 56 words

The process as claimed in claim 11 in which the interhalogen compound is a member selected from the group consisting of ClF, BrF, IF, BrCl, ICl, IBr, ClF 3 , BrF 3 , IF 3 , ICl 3 or I 2 Cl 6 , ClF 5 , BrF 5 , IF 5 and IF 7 .

Claim 14

Dependent Claim 25 words

The process as claimed in claim 12 in which the interhalogen compound is a member selected from the group consisting of ICl 3 and ICl.

Claim 15

Dependent Claim 41 words

The process as claimed in claim 1 in which the treatment with the interhalogen compound is carried out in the presence of a diluent at a temperature of from room temperature to 150° C. for from 30 minutes to 10 hours.

Claim 16

Dependent Claim 15 words

The process as claimed in claim 14 in which the diluent is a halogenated hydrocarbon.

Claim 17

Dependent Claim 26 words

The process as claimed in claim 1 in which the interhalogen is in a quantity of 0.005 to 0.1 mole per mole of the titanium trichloride.

Claim 18

Dependent Claim 41 words

The process as claimed in claim 1 in which the titanium tetrachloride composition having a β-crystal structure is heat treated at a temperature of about 150° to 180° C. under an atmosphere of an inert gas for 1 to 10 hours.

Claim 19

Dependent Claim 31 words

A process as claimed in claim 1 in which said titanium trichloride is heat treated to transform said titanium trichloride having a β-crystal structure into titanium trichloride having a γ-crystal structure.

Claim 20

Dependent Claim 38 words

A process as claimed in claim 1 in which said titanium trichloride is heat treated so as to transform said titanium trichloride having a β-crystal structure into titanium trichloride having a γ-crystal structure containing substantially no β-crystal structure.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1982-04-23	1982-10-23	1983-04-24	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1986-04-23	1986-10-23	1987-04-24	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1990-04-23	1990-10-23	1991-04-24	$7700.00	Window Closed / Lapsed

Process for preparing titanium trichloride compositions

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