US4316852A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Manufacture of metallic soaps
Assignee: HL Blachford Ltd
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Filing: 1980-03-13
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Granted: 1982-02-23
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Expires: 2000-03-13
Abstract
Abstract Metallic soaps, particularly zinc soaps are produced from a reaction mixture initially comprising a metal oxide or hydroxide, for example, zinc oxide, water and a glyceryl ester, particularly a triglyceride, the ester and said metal oxide or hydroxide being present in at least approximately stoichiometric amounts; the reaction mixture is agitated and the reactants are reacted in the agitated mixture to produce a metallic soap and glycerine, at a temperature at which the metallic soap is molten, in the presence of an excess of water effective to dissolve the glycerine formed in the reaction mixture such that reaction between by-product glycerine and the product metallic soap is substantially hindered, eventually the reaction mixture is allowed to separate into an aqueous layer and a molten layer of product metallic soap under a pressure such that the aqueous layer is essentially quiescent, and the molten metallic soap layer is dissociated from the aqueous layer; in this way metallic soaps of high purity can be obtained.
Inventors
- 👤 John Blachford
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 19:34
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/41; C07C51/412
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
327 words
A process for producing a metallic soap having a viscosity such that it is a pourable liquid when molten, of a monocarboxylic acid of the formula R-COOH wherein R is a linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated aliphatic hydrocarbon radical of 5 to 21 carbon atoms, which comprises: (i) forming a reaction mixture initially comprising a metal component comprising a metal oxide selected from the group consisting of oxides of cadmium, lead and zinc or a metal hydroxide selected from the group consisting of hydroxides of cobalt, manganese, and zinc, water and a glyceryl ester of formula (I): H.sub.2 C(OR.sub.1)CH(OR.sub.2)CH.sub.2 (OR.sub.3) (I) wherein R 1 , R 2 and R 3 , which may be the same or different, are selected from the group consisting of hydrogen and linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated aliphatic hydrocarbon acyl radicals of 6 to 22 carbon atoms, provided that at least one of R 1 , R 2 and R 3 is an acyl radical, said ester and said metal oxide or hydroxide being present in at least approximately stoichiometric amounts, (ii) agitating said reaction mixture, (iii) reacting the reactants in the agitated mixture to produce a metallic soap and glycerine, at a temperature at which the metallic soap is molten, in the presence of an excess of water effective to dissolve the glycerine formed in the reaction mixture such that reaction between by-product glycerine and the product metallic soap is substantially hindered, (iv) continuing said reacting in (iii) until substantially no more metallic soap is formed, (v) allowing the reaction mixture to separate into an aqueous layer and a molten layer of product metallic soap substantially free of metallic oxide or metallic hydroxide, carboxylic acid and glyceryl ester, under a pressure such that said aqueous layer is essentially quiescent, and (vi) dissociating the molten metallic soap layer from the aqueous layer.
Claim 2
Dependent Claim
327 words
A process for producing a metallic soap having a viscosity such that it is a pourable liquid when molten, of a monocarboxylic acid of the formula R-COOH wherein R is a linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated aliphatic hydrocarbon radical of 5 to 21 carbon atoms, which comprises: (i) forming a reaction mixture initially comprising a metal component comprising a metal oxide selected from the group consisting of oxides of cadmium, lead and zinc or a metal hydroxide selected from the group consisting of hydroxides of cobalt, manganese, and zinc, water and a glyceryl ester of formula (I): H.sub.2 C(OR.sub.1)CH(OR.sub.2)CH.sub.2 (OR.sub.3) (I) wherein R 1 , R 2 and R 3 , which may be the same or different, are selected from the group consisting of hydrogen and linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated aliphatic hydrocarbon acyl radicals of 6 to 22 carbon atoms, provided that at least one of R 1 , R 2 and R 3 is an acyl radical, said ester and said metal oxide or hydroxide being present in at least approximately stoichiometric amounts, (ii) agitating said reaction mixture, (iii) reacting the reactants in the agitated mixture to produce a metallic soap and glycerine, at a temperature at which the metallic soap is molten, in the presence of an excess of water effective to dissolve the glycerine formed in the reaction mixture such that reaction between by-product glycerine and the product metallic soap is substantially hindered, (iv) continuing said reacting in (iii) until substantially no more metallic soap is formed, (v) allowing the reaction mixture to separate into an aqueous layer and a molten layer of product metallic soap substantially free of metallic oxide or metallic hydroxide, carboxylic acid and glyceryl ester, under a pressure such that said aqueous layer is essentially quiescent, and (vi) dissociating the molten metallic soap layer from the aqueous layer.
Claim 3
Dependent Claim
24 words
A process according to claim 1, wherein said metal component is selected from the group consisting of cadmium oxide, lead oxide and zinc oxide.
Claim 4
Dependent Claim
15 words
A process according to claim 2, wherein said glyceryl ester is a mono- or diglyceride.
Claim 5
Dependent Claim
13 words
A process according to claim 1, wherein said glyceryl ester is a triglyceride.
Claim 6
Dependent Claim
13 words
A process according to claim 2, wherein said glyceryl ester is a triglyceride.
Claim 7
Dependent Claim
20 words
A process according to claim 1, wherein said metal component is zinc oxide and the glyceryl ester is a triglyceride.
Claim 8
Dependent Claim
17 words
A process according to claim 6, wherein the triglyceride is prepared by hydrogenating a naturally occurring triglyceride.
Claim 9
Dependent Claim
18 words
A process according to claim 1, wherein said reaction in (iii) is continued for 0.5 to 10 hours.
Claim 10
Dependent Claim
34 words
A process according to claim 1, in which said reaction mixture contains at least as much water by weight as the amount by weight of glycerine that would be produced in reacting to completion.
Claim 11
Dependent Claim
31 words
A process according to claim 2, wherein said glyceryl ester comprises a mixture of at least two esters selected from the group consisting of monoglycerides, diglycerides and triglycerides of formula (I).
Claim 12
Dependent Claim
261 words
A process for producing a zinc soap having a viscosity of less than 500,000 centipoise when molten, which comprises: (i) forming a reaction mixture initially comprising zinc oxide, water and a triglyceride in which the molar ratio of the triglyceride to the zinc oxide is about 2:3, (ii) agitating said reaction mixture, (iii) reacting the reactants in the agitated mixture to produce a zinc soap and glycerine, at a temperature at which the metallic soap is molten, in accordance with the equation (II): 2H.sub.2 C(OR.sub.1)CH(OR.sub.2)CH.sub.2 (OR.sub.3)+3ZnO+3H.sub.2 O→2CH.sub.2 OHCHOHCH.sub.2 OH+3R.sub.4 OZnOR.sub.5 (II) wherein R 1 , R 2 and R 3 , which may be the same or different, are selected from the group consisting of linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated, aliphatic hydrocarbon acyl radicals of 6 to 22 carbon atoms and R 4 and R 5 , which may be the same or different, are acyl radicals selected from R 1 , R 2 and R 3 , in the presence of an excess of water effective to dissolve the glycerine formed in the reaction mixture such that reaction between the by-product glycerine and the product zinc soap is substantially hindered, (iv) continuing said reaction to at least 95% completion, (v) allowing the reaction mixture to separate into an aqueous layer and a molten layer of zinc soap substantially free of zinc oxide, carboxylic acid and glyceryl ester, under a pressure such that said aqueous layer is essentially quiescent, and (vi) dissociating the molten zinc soap layer from the aqueous layer.
Claim 13
Dependent Claim
261 words
A process for producing a zinc soap having a viscosity of less than 500,000 centipoise when molten, which comprises: (i) forming a reaction mixture initially comprising zinc oxide, water and a triglyceride in which the molar ratio of the triglyceride to the zinc oxide is about 2:3, (ii) agitating said reaction mixture, (iii) reacting the reactants in the agitated mixture to produce a zinc soap and glycerine, at a temperature at which the metallic soap is molten, in accordance with the equation (II): 2H.sub.2 C(OR.sub.1)CH(OR.sub.2)CH.sub.2 (OR.sub.3)+3ZnO+3H.sub.2 O→2CH.sub.2 OHCHOHCH.sub.2 OH+3R.sub.4 OZnOR.sub.5 (II) wherein R 1 , R 2 and R 3 , which may be the same or different, are selected from the group consisting of linear or branched, unsubstituted or substituted by one or more hydroxyl groups, saturated or unsaturated, aliphatic hydrocarbon acyl radicals of 6 to 22 carbon atoms and R 4 and R 5 , which may be the same or different, are acyl radicals selected from R 1 , R 2 and R 3 , in the presence of an excess of water effective to dissolve the glycerine formed in the reaction mixture such that reaction between the by-product glycerine and the product zinc soap is substantially hindered, (iv) continuing said reaction to at least 95% completion, (v) allowing the reaction mixture to separate into an aqueous layer and a molten layer of zinc soap substantially free of zinc oxide, carboxylic acid and glyceryl ester, under a pressure such that said aqueous layer is essentially quiescent, and (vi) dissociating the molten zinc soap layer from the aqueous layer.
Claim 14
Dependent Claim
59 words
A process according to claim 11, wherein said temperature in (iii) is about 175° to 195° C., said reacting is carried out from 2 to 5 hours and said reaction mixture in (i) comprises water in an amount by weight of about 2 to about 7 times the stoichiometric amount by weight of glycerine produced according to equation (II).
Claim 15
Dependent Claim
48 words
A process according to claim 12, wherein step (v) includes introducing an inert gas to maintain a pressure above the reaction mixture above the vapour pressure of aqueous glycerine in the product reaction mixture, whereby boiling of the aqueous glycerine is prevented and said separate layers are formed.
Claim 16
Dependent Claim
23 words
A process according to claim 13, wherein said zinc oxide in said reaction mixture has a particle size not greater than 45 microns.
Claim 17
Dependent Claim
28 words
A process according to claim 13, wherein said agitating in (ii) is effective to disperse said triglyceride as small droplets having a size of 1 to 1,000 microns.
Claim 18
Dependent Claim
26 words
A process according to claim 15, wherein mono- and diglycerides are produced as intermediates in said reacting effective to maintain the small droplet size of triglycerides.
Claim 19
Dependent Claim
12 words
A process according to claim 14, wherein said triglyceride is hydrogenated tallow.
Claim 20
Dependent Claim
16 words
A process according to claim 14, wherein said triglyceride has an iodine value less than 10.
Claim 21
Dependent Claim
49 words
A process according to claim 13, wherein after step (iv) and prior to step (v) there is included a step of establishing a difference in density between the molten zinc soap and the aqueous glycerine, whereby the aqueous layer and the molten soap layer may form in step (v).
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) | 1985-02-22 | 1985-08-24 | 1986-02-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-02-22 | 1989-08-24 | 1990-02-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-02-22 | 1993-08-24 | 1994-02-23 | $7700.00 | Window Closed / Lapsed |