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US4029747A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of preparing inorganic monomeric and polymeric complexes and products so produced

Assignee: Molecular Energy Research Co Inc
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Filing: 1975-11-17
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Granted: 1977-06-14
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Expires: 1995-11-17
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Abstract

Abstract Novel water soluble, inorganic complexes are obtained by reacting, in the presence of aqueous ammonia, at least one non-alkaline metal selected from Groups I-VIII of the Periodic Table with an alkali metal hydroxide. An excess of the non-alkaline metal or metals is introduced into a reaction vessel, preferably already containing the aqueous ammonia, and the alkali metal hydroxide is thereafter incrementally added in such manner as to create localized areas of high concentration and pH approaching a value of 14. The hydrooxide in these areas of high concentration, in combination with reactive NH2 groups provided by the aqueous ammonia, causes erosion of the non-alkaline metal, the formation of non-alkaline metal ions and the production of a monomeric, metal amide complex. The reaction parameters are maintained such that the rate of addition of alkali metal hydroxide is sufficient to suppress the expulsion from the system of ammonia gas while at the same time producing an overall endothermic reaction in which the ions of the alkali metal, the non-alkaline metal and the NH2 groups react to produce an inorganic complex. If the endothermic reaction is maintained and sufficient excess non-alkaline metal is present in the aqueous medium, after a period of time the reaction will enter an exothermic phase, producing an inorganic polymeric complex which remains soluble in water throughout a substantial molecular weight range.

Inventors

  • 👤 George G. Merkl

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 21:39
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/082; C01B21/087; C01B21/092; C01B21/0923; C01B21/0926

Claims Analysis

Total Claims: 29
Claim 1
Independent Claim 243 words
A method of producing an inorganic polymeric complex which comprises: reacting in an aqueous medium a. at least one non-alkaline metal selected from Groups I-VIII of the Periodic Table; b. an alkali metal hydroxide; and c. a source of reactive NH 2 groups according to the following sequence: i. introducing a predetermined quantity of said non-alkaline metal into a reaction vessel containing said aqueous medium; ii. providing in said aqueous medium, a supply of said source of NH 2 groups; iii. adding said alkali metal hydroxide to said reaction vessel, in the present of said source of NH 2 groups, in such manner as to provide intimate contact between the alkali metal ions and the non-alkaline metal and a localized area in the immediate vicinity of said non-alkaline metal of pH approaching a value of 14, whereby the non-alkaline metal erodes, producing non-alkaline metal ions in said reaction medium, said non-alkaline metal ions entering into reaction with the alkali metal ions and reactive NH 2 groups to produce an inorganic monomeric complex; said alkali metal hydroxide being added at a rate sufficient to bind substantial quantities of NH 2 in an overall endothermic reaction with said alkali metal hydroxide and said non-alkaline metal; iv. thereafter establishing an exothermic reaction in said reaction vessel characterized by increased erosion of said non-alkaline metal and the formation of an inorganic polymeric complex; and terminating the reaction by removing any unreacted non-alkaline metal from the reaction medium.
Claim 2
Independent Claim 243 words
A method of producing an inorganic polymeric complex which comprises: reacting in an aqueous medium a. at least one non-alkaline metal selected from Groups I-VIII of the Periodic Table; b. an alkali metal hydroxide; and c. a source of reactive NH 2 groups according to the following sequence: i. introducing a predetermined quantity of said non-alkaline metal into a reaction vessel containing said aqueous medium; ii. providing in said aqueous medium, a supply of said source of NH 2 groups; iii. adding said alkali metal hydroxide to said reaction vessel, in the present of said source of NH 2 groups, in such manner as to provide intimate contact between the alkali metal ions and the non-alkaline metal and a localized area in the immediate vicinity of said non-alkaline metal of pH approaching a value of 14, whereby the non-alkaline metal erodes, producing non-alkaline metal ions in said reaction medium, said non-alkaline metal ions entering into reaction with the alkali metal ions and reactive NH 2 groups to produce an inorganic monomeric complex; said alkali metal hydroxide being added at a rate sufficient to bind substantial quantities of NH 2 in an overall endothermic reaction with said alkali metal hydroxide and said non-alkaline metal; iv. thereafter establishing an exothermic reaction in said reaction vessel characterized by increased erosion of said non-alkaline metal and the formation of an inorganic polymeric complex; and terminating the reaction by removing any unreacted non-alkaline metal from the reaction medium.
Claim 3
Dependent Claim 15 words
The method of claim 1, wherein said source of NH 2 groups is aqueous ammonia.
Claim 4
Dependent Claim 19 words
The method of claim 2, wherein said aqueous ammonia is provided by bubbling gaseous ammonia through said aqueous medium.
Claim 5
Dependent Claim 14 words
The method of claim 2, wherein said aqueous ammonia is supplemented with ammonia gas.
Claim 6
Dependent Claim 27 words
The method of claim 1, wherein the exothermic reaction is initiated by heating the reaction vessel containing the inorganic monomeric complex following completion of the endothermic reaction.
Claim 7
Dependent Claim 25 words
The method of claim 1, wherein the exothermic reaction is initiated by adding additional non-alkaline metal to the reaction vessel containing the inorganic monomeric complex.
Claim 8
Dependent Claim 27 words
The method of claim 1, wherein the reaction is cooled during the addition of the alkali metal hydroxides to assist in the development of the endothermic reaction.
Claim 9
Dependent Claim 44 words
The method of claim 1, further including adding to the reaction vessel a small quantity of non-alkaline metal of a different non-alkaline metal of groups I-VIII of the periodic table, more reactive than said non-alkaline metal, to initiate the development of said endothermic reaction.
Claim 10
Dependent Claim 49 words
The method of claim 1, wherein the more reactive metal comprises the same non-alkaline metal of groups I-VIII of the periodic table, previously utilized in reaction with an alkali metal hydroxide and a source of reactive NH 2 groups through the exothermic reaction to produce the inorganic polymeric complex.
Claim 11
Dependent Claim 18 words
The method of claim 1, wherein said alkali metal hydroxide is selected from sodium hydroxide and potassium hydroxide.
Claim 12
Dependent Claim 45 words
The method of claim 1, wherein the alkali metal hydroxide is added to the reaction vessel in pellet form, the pellets sinking to the bottom of the reaction vessel proximate to the non-alkaline metal and producing said localized areas of high pH as they dissolve.
Claim 13
Dependent Claim 47 words
The method of claim 1, wherein said source of NH 2 groups comprises ammonia gas, said ammonia gas and alkali metal hydroxide being added to said reaction medium under controlled conditions so as to bind a substantial quantity of NH 2 groups released from the ammonia gas.
Claim 14
Dependent Claim 11 words
The method of claim 1, wherein said non-alkaline metal is silicon.
Claim 15
Dependent Claim 11 words
The method of claim 1, wherein said non-alkaline metal is aluminum.
Claim 16
Dependent Claim 14 words
The aqueous solution of inorganic polymeric complex produced by the method of claim 1.
Claim 17
Independent Claim 212 words
A method which comprises: reacting in an aqueous medium a. at least one non-alkaline metal selected from Groups I-VIII of the Periodic Table; b. an alkali metal hydroxide; and c. a source of reactive NH 2 groups according to the following sequence: i. introducing a predetermined quantity of said non-alkaline metal into a reaction vessel containing said aqueous medium; ii. providing, in said aqueous medium, a supply of said source of NH 2 groups; iii. adding said alkali metal hydroxide to said reaction vessel, in the presence of said source of NH 2 groups, in such manner as to provide intimate contact between the alkali metal ions and the non-alkaline metal and a localized area in the immediate vicinity of said non-alkaline metal of pH approaching a value of 14, whereby the non-alkaline metal erodes, producing non-alkaline metal ions in said reaction medium, said non-alkaline metal ions entering into reaction with the alkali metal ions and reactive NH 2 groups to produce an inorganic monomeric complex; said alkaline metal hydroxide being added at a rate sufficient to bind substantial quantities of NH 2 groups in an overall endothermic reaction with said alkali metal hydroxide and said non-alkaline metal; and terminating the reaction by removing any unreacted non-alkaline metal from the reaction medium.
Claim 18
Independent Claim 212 words
A method which comprises: reacting in an aqueous medium a. at least one non-alkaline metal selected from Groups I-VIII of the Periodic Table; b. an alkali metal hydroxide; and c. a source of reactive NH 2 groups according to the following sequence: i. introducing a predetermined quantity of said non-alkaline metal into a reaction vessel containing said aqueous medium; ii. providing, in said aqueous medium, a supply of said source of NH 2 groups; iii. adding said alkali metal hydroxide to said reaction vessel, in the presence of said source of NH 2 groups, in such manner as to provide intimate contact between the alkali metal ions and the non-alkaline metal and a localized area in the immediate vicinity of said non-alkaline metal of pH approaching a value of 14, whereby the non-alkaline metal erodes, producing non-alkaline metal ions in said reaction medium, said non-alkaline metal ions entering into reaction with the alkali metal ions and reactive NH 2 groups to produce an inorganic monomeric complex; said alkaline metal hydroxide being added at a rate sufficient to bind substantial quantities of NH 2 groups in an overall endothermic reaction with said alkali metal hydroxide and said non-alkaline metal; and terminating the reaction by removing any unreacted non-alkaline metal from the reaction medium.
Claim 19
Dependent Claim 15 words
The method of claim 16, wherein said source of NH 2 groups is aqueous ammonia.
Claim 20
Dependent Claim 19 words
The method of claim 17, wherein said aqueous ammonia is provided by bubbling gaseous ammonia through said aqueous medium.
Claim 21
Dependent Claim 14 words
The method of claim 17, wherein said aqueous ammonia is supplemented with ammonia gas.
Claim 22
Dependent Claim 27 words
The method of claim 16, wherein the reaction is cooled during the addition of the alkali metal hydroxide to assist in the development of the endothermic reaction.
Claim 23
Dependent Claim 45 words
The method of claim 16, further including adding to the reaction vessel a small quantity of a non-alkaline metal of a different non-alkaline metal of groups I-VIII of the periodic table, more reactive than said non-alkaline metal, to initiate the development of said endothermic reaction.
Claim 24
Dependent Claim 18 words
The method of claim 16, wherein said alkali metal hydroxide is selected from sodium hydroxide and potassium hydroxide.
Claim 25
Dependent Claim 44 words
The method of claim 16, wherein the alkali metal hydroxide is added to the reaction vessel in pellet form, the pellets sinking to the bottom of the reaction proximate to the non-alkaline metal and producing said localized areas of high pH as they dissolve.
Claim 26
Dependent Claim 47 words
The method of claim 16, wherein said source of NH 2 groups comprises ammonia gas, said ammonia gas and alkali metal hydroxide being added to said reaction medium under controlled conditions so as to bind a substantial quantity of NH 2 groups released from the ammonia gas.
Claim 27
Dependent Claim 11 words
The method of claim 16, wherein said non-alkaline metal is silicon.
Claim 28
Dependent Claim 11 words
The method of claim 16, wherein said non-alkaline metal is aluminum.
Claim 29
Dependent Claim 14 words
The aqueous solution of inorganic monomeric complex produced by the method of claim 16.

References Cited (Backward Citations)

CA586843A Cited
GB191225891A Cited
FR510631A Cited
CH76038A Cited
US2163100A Cited
US2202994A Cited
US2971988A Cited
US3350172A Cited
US3797238A Cited
US3523047A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-06-13 1980-12-13 1981-06-14 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-06-13 1984-12-13 1985-06-14 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-06-13 1988-12-13 1989-06-14 $7700.00 Window Closed / Lapsed

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