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US3687994A
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Method of manufacturing alkylaluminum compounds
Assignee: Ethyl Corp
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Filing: 1970-12-16
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Granted: 1972-08-29
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Expires: 1990-12-16
Abstract
Abstract A method of manufacturing alkylaluminum compounds from ternary or quaternary alloys, comprising as principal elements aluminum, silicon and titanium, and aluminum, silicon, titanium and iron, respectively, wherein said alloys are reacted with hydrogen and an aluminum alkyl. An olefin and/or a catalyst may also be added in the reaction.
Inventors
- 👤 Paul Kobetz
- 👤 Warren E Becker
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 13:50
CPC Classifications
C; C22; C22C; C22C21/00; C22C21/02; C07; C07F; C07F5/00; C07F5/06; C07F5/061; C07F5/065
Claims Analysis
Total Claims: 40
Claim 1
Independent Claim
31 words
The method of claim 1, wherein said aluminum-silicon alloy is a quaternary alloy comprising 0.6 to 3 percent by weight of titanium, and 1 to 4 percent by weight of iron.
Claim 2
Dependent Claim
18 words
A method according to claim 1, wherein said reaction is effected at a temperature between 70*C and 250*C.
Claim 3
Dependent Claim
18 words
A method according to claim 1, wherein said reaction is effected at a temperature between 100*C and 180*C.
Claim 4
Dependent Claim
77 words
A method according to claim 1, wherein said catalyst has the formula MYn.Al(C2H5)RX, wherein M is an alkali metal or alkaline earth metal; Y is hydrogen, chlorine, fluorine, hydroxyl group, cyanide group, alkyl group or alkoxy group; n is an integer in accordance with the valences of M and Y; R is hydrogen or a hydrocarbyl group having up to 20 carbon atoms; and X is hydrogen, halogen or hydrocarbyl group having up to twenty carbon atoms.
Claim 5
Dependent Claim
19 words
A method according to claim 1, wherein said catalyst is a sodium alkylaluminum compound or a sodium alkyl-aluminum hydride.
Claim 6
Dependent Claim
85 words
A method according to claim 1, wherein said catalyst has the general formula of RnMy wherein R is a member selected from the group consisting of alkoxy, aroxy, alkaroxy, aralkoxy, alkyl, aryl, aralkyl and alkaryl radicals, Y is a member selected from the group consisting of alkoxy, aroxy, aralkoxy and alkaroxy radicals, M is a metal element selected from the group consisting of lithium, sodium, potassium and magnesium and n is 0 when M is sodium, potassium or lithium and 1 when M is magnesium.
Claim 7
Dependent Claim
21 words
A method according to claim 1, wherein said catalyst is selected from the group consisting of sodium metal and sodium hydride.
Claim 8
Independent Claim
176 words
A method of making alkylaluminum compounds comprising: reacting a ternary or quaternary aluminum alloy, comprising by weight 33 to 94 percent aluminum, 5 to 58 percent silicon, 0.2 to 4 percent titanium and up to 5 percent iron, with a mixture selected from the group consisting of an alkylaluminum compounD and hydrogen or an alkylaluminum compound, hydrogen and an olefin, the said alkylaluminum compound having the general formula of RR''AlR''''; wherein R and R'' are alkyl radicals having from two to 20 carbon atoms, and R'''' is an alkyl radical or in the presence of an olefin, hydrogen; in the presence of a catalyst or activating agent having the general formula MYn.Al(C2H5)RX, wherein M is an alkali metal or alkaline earth metal; Y is hydrogen, chlorine, fluorine, hydroxyl group, cyanide group, alkyl group or alkoxy group; n is an integer in accordance with the valences of M and Y; R is hydrogen or a hydrocarbyl group having up to 20 carbon atoms; and X is hydrogen, halogen or hydrocarbyl group having up to 20 carbon atoms.
Claim 9
Dependent Claim
33 words
The method of claim 9, wherein the titanium in said quaternary alloy is 0.6 to 3 percent by weight and the iron in said quaternary alloy is 1 to 4 percent by weight.
Claim 10
Dependent Claim
18 words
A method according to claim 9, wherein said olefin is an alpha-olefin having 2 to twenty carbon atoms.
Claim 11
Dependent Claim
18 words
A method according to claim 9, wherein said reaction is effected at a temperature between 70*C and 250*C.
Claim 12
Dependent Claim
18 words
A method according to claim 9, wherein said reaction is effected at a temperature between 100*C and 180*C.
Claim 13
Dependent Claim
20 words
The method of claim 9, wherein the alkali metal is selected from the group consisting of sodium, potassium or lithium.
Claim 14
Dependent Claim
20 words
The method of claim 9, wherein the alkaline earth metal is selected from the group consisting of calcium or magnesium.
Claim 15
Dependent Claim
15 words
The method of claim 9, wherein the catalyst or activating agent is sodium ethylaluminum hydride.
Claim 16
Dependent Claim
15 words
The method of claim 9, wherein the reaction is conducted in an inert hydrocarbon medium.
Claim 17
Dependent Claim
18 words
The method of claim 9, wherein when an olefin is reacted, the olefin contains catalytic amounts of ethylene.
Claim 18
Dependent Claim
28 words
The method of claim 9, wherein the alkylaluminum compound is a member selected from the group consisting of triethylaluminum, di-n-propyaluminum hydride, tri-n-propylaluminum, triisobutylaluminum, diisobutylaluminum hydride and mixtures thereof.
Claim 19
Independent Claim
45 words
A method for producing alkylaluminum compounds which comprises reacting an aluminum-silicon ternary alloy containing as the third principal element titanium in an amount sufficient to speed up the reaction, with an alkylaluminum compound, hydrogen and a catalyst containing an alkali metal or alkaline earth metal.
Claim 20
Dependent Claim
17 words
The method of claim 20, wherein said reaction is carried out in the presence of an olefin.
Claim 21
Dependent Claim
18 words
The method of claim 21, wherein said olefin is an alpha-olefin having from 2 to twenty carbon atoms.
Claim 22
Dependent Claim
35 words
The method of claim 20, wherein said ternary alloy consists essentially of 33 to 94 percent by weight of aluminum, 5 to 58 percent by weight of silicon and 0.2-4 percent by weight of titanium.
Claim 23
Dependent Claim
21 words
The method of claim 23, wherein the amount of titanium in said ternary alloy is 0.6 to 3 percent by weight.
Claim 24
Dependent Claim
76 words
The method of claim 20, wherein said catalyst has the formula MYn.Al(C2H5)RX, wherein M is an alkali metal or alkaline earth metal; Y is hydrogen, chlorine, fluorine, hydroxyl group, cyanide group, alkyl group or alkoxy group; n is an integer in accordance with the valences of M and Y; R is hydrogen or a hydrocarbyl group having up to 20 carbon atoms; and X is hydrogen, halogen or hydrocarbyl group having up to twenty carbon atoms.
Claim 25
Independent Claim
68 words
A method for producing alkylaluminum compounds, which comprises reacting a quaternary alloy comprising 33 to 94 percent by weight of aluminum, 5 to 58 percent by weight of silicon, 1 to 5 percent by weight of iron, and 0.2 percent to 4 percent by weight of titanium, with a catalyst containing an alkali metal or alkaline earth metal, an aluminum alkyl compound and hydrogen at an elevated temperature.
Claim 26
Dependent Claim
27 words
The method of claim 26, wherein said quaternary alloy comprises 0.6 to 3 percent by weight of aluminum and 1 to 4 percent by weight of iron.
Claim 27
Dependent Claim
17 words
The method of claim 26, wherein said reaction is carried out in the presence of an olefin.
Claim 28
Dependent Claim
18 words
The method of claim 28, wherein said olefin is an alpha-olefin having from 2 to twenty carbon atoms.
Claim 29
Dependent Claim
19 words
The method of claim 26, wherein the reaction is conducted at a temperature from about 70*C to about 250*C.
Claim 30
Dependent Claim
15 words
The method of claim 26, wherein the catalyst or activating agent is sodium ethylaluminum hydride.
Claim 31
Dependent Claim
16 words
The method of claim 26, wherein the reaction is carried out in an inert hydrocarbon medium.
Claim 32
Dependent Claim
18 words
The method of claim 26, wherein when an olefin is reacted, the olefin contains catalytic amounts of ethylene.
Claim 33
Dependent Claim
49 words
In a process of preparing aluminum alkyl from aluminum in the presence of hydrogen and an aluminum alkyl, the improvement wherein the aluminum is employed in the form of an aluminum-silicon-iron-titanium alloy containing at least some metallic aluminum not held in the tightly bound form of an intermetallic compound.
Claim 34
Dependent Claim
17 words
The process of claim 34 further characterized in being performed in the additional presence of an alpha-olefin.
Claim 35
Dependent Claim
27 words
The process of claim 34 further characterized in being performed in the additional presence of an alpha-olefin selected from the group consisting of ethylene, propylene and isobutylene.
Claim 36
Dependent Claim
74 words
In a process of preparing aluminum alkyl from aluminum in the presence of hydrogen and an aluminum alkyl at an elevated temperature and pressure, the improvement wherein the source of the aluminum for the reaction is an aluminum-silicon-iron-titanium alloy which contains at least about 3 weight percent iron, at least about 2 weight percent titanium, and at least some metallic aluminum which is not held in the tightly bound form of an intermetallic compound.
Claim 37
Dependent Claim
19 words
The process of claim 37 further characterized in being performed in the additional presence of ethylene, propylene, or isobutylene.
Claim 38
Dependent Claim
33 words
The process of claim 37 further characterized in that said alloy contains about 68 weight percent aluminum, about 27 weight percent silicon, about 3 weight percent iron and about 2 weight percent titanium.
Claim 39
Dependent Claim
67 words
In a process of preparing alkylaluminum from aluminum in the presence of hydrogen, an aluminum alkyl, and a relatively small amount of sodium or sodium hydride to enhance the reactivity of the system, the improvement wherein the aluminum is employed in the form of an aluminum-silicon-iron-titanium alloy which contains at least some metallic aluminum which is not held in the tightly bound form of an intermetallic compound.
Claim 40
Dependent Claim
19 words
The process of claim 40 further characterized in being performed in the additional presence of ethylene, propylene, or isobutylene.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1975-08-29 | 1976-02-28 | 1976-08-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-08-29 | 1980-02-28 | 1980-08-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-08-29 | 1984-02-28 | 1984-08-29 | $7700.00 | Window Closed / Lapsed |