US4263145A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Recovery of ammonia or amine from a cation exchange resin
Assignee: Dow Chemical Co
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Filing: 1980-06-10
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Granted: 1981-04-21
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Expires: 2000-06-10
Abstract
Abstract Ammonia or an amine such as morpholine is recovered from a resin bed comprising an alkali metal, e.g., sodium, and ammonium or amine salts of a strong acid cation exchange resin by contacting the cation resin with an aqueous solution of an alkaline earth metal hydroxide, e.g., calcium hydroxide, thereby exchanging the alkali metal and ammonium or amine cations with alkaline earth metal cations. The aqueous liquid containing the alkali metal and ammonia or amine is subsequently passed through a cation exchange resin which removes the alkali metal from the liquid. The recovery of ammonia or the amine by such method is particularly useful in condensate purification system associated with a power production facility wherein the recovered ammonia or amine can be employed to reduce corrosion in the power production facility and the strong acid resin, upon regeneration, can be used to remove alkali metal ions, particularly sodium, from the facility.
Inventors
- 👤 Louis F. Wirth, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 08:16
CPC Classifications
B; B01; B01J; B01J47/00; B01J47/02; B01J47/04; B01J39/00; B01J39/04; B01J39/05; B01J49/00; B01J49/05; B01J49/06
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
126 words
A method for recovering ammonia or an amine from a strong acid cation exchange resin having both an alkali metal and ammonium or the amine cations attached thereto, said method comprising the steps of: (a) exchanging the alkali metal and ammonium or amine cations on the strong acid cation resin with alkaline earth metal cations by contacting the resin with an aqueous liquid containing alkaline earth metal cations at conditions sufficient to form an aqueous solution of hydroxides of the alkali metal and ammonia or amine and (b) subsequently contacting the resulting aqueous solution containing the hydroxides of the alkali metal and ammonia or amine with a cation exchange resin at conditions such that the concentration of the alkali metal in the solution is selectively reduced.
Claim 2
Independent Claim
126 words
A method for recovering ammonia or an amine from a strong acid cation exchange resin having both an alkali metal and ammonium or the amine cations attached thereto, said method comprising the steps of: (a) exchanging the alkali metal and ammonium or amine cations on the strong acid cation resin with alkaline earth metal cations by contacting the resin with an aqueous liquid containing alkaline earth metal cations at conditions sufficient to form an aqueous solution of hydroxides of the alkali metal and ammonia or amine and (b) subsequently contacting the resulting aqueous solution containing the hydroxides of the alkali metal and ammonia or amine with a cation exchange resin at conditions such that the concentration of the alkali metal in the solution is selectively reduced.
Claim 3
Dependent Claim
39 words
The method of claim 1 wherein the exchange of the alkali metal and ammonium or amine cations on the strong acid cation resin is conducted by contacting the resin with an aqueous solution of an alkaline earth metal hydroxide.
Claim 4
Dependent Claim
14 words
The method of claim 2 wherein the alkaline earth metal hydroxide is calcium hydroxide.
Claim 5
Dependent Claim
26 words
The method of claim 3 wherein the aqueous solution of the alkaline earth metal hydroxide comprises from about 0.1 to about 0.12 weight percent calcium hydroxide.
Claim 6
Dependent Claim
64 words
The method of claim 1 wherein the exchange of the alkali metal and ammonium or amine cations on the strong acid cation resin is conducted by contacting the resin with an aqueous salt solution of an alkaline earth metal and subsequently contacting the resulting aqueous liquid containing salts of the alkali metal and ammonia or amine with a strong base resin in hydroxide form.
Claim 7
Dependent Claim
27 words
The method of claim 5 wherein the aqueous salt solution of an alkaline earth metal is an aqueous solution of a water-soluble salt of calcium or magnesium.
Claim 8
Dependent Claim
17 words
The method of claim 6 wherein the water-soluble salt is calcium chloride, magnesium chloride or magnesium sulfate.
Claim 9
Dependent Claim
30 words
The method of claim 7 wherein the aqueous salt solution of an alkaline earth metal comprises from about 0.5 to about 10 weight percent of the alkaline earth metal salt.
Claim 10
Dependent Claim
166 words
An improved method for purifying condensate containing alkali metal and ammonium or amine cations, the method comprising the steps of: (a) contacting the condensate with a resin bed comprising a strong acid cation exchange resin thereby converting the cation exchange resin to salts of an alkali metal and ammonium or amine; and (b) regenerating the cation resin, the improvement in said method comprising the steps of: (c) exchanging the alkali metal and ammonium or amine cations attached to the cation resin, prior to the regeneration thereof, with alkaline earth metal cations, thereby converting the cation resin to alkaline earth metal form, by contacting said resin with an aqueous liquid containing alkaline earth metal cations at conditions sufficient to form an aqueous solution of hydroxides of the alkali metal and ammonium or amine; and (d) contacting the aqueous hydroxide solution of the alkali metal and ammonia or amine with a cation exchange resin at conditions sufficient to selectively remove essentially all the alkali metal from the liquid.
Claim 11
Dependent Claim
166 words
An improved method for purifying condensate containing alkali metal and ammonium or amine cations, the method comprising the steps of: (a) contacting the condensate with a resin bed comprising a strong acid cation exchange resin thereby converting the cation exchange resin to salts of an alkali metal and ammonium or amine; and (b) regenerating the cation resin, the improvement in said method comprising the steps of: (c) exchanging the alkali metal and ammonium or amine cations attached to the cation resin, prior to the regeneration thereof, with alkaline earth metal cations, thereby converting the cation resin to alkaline earth metal form, by contacting said resin with an aqueous liquid containing alkaline earth metal cations at conditions sufficient to form an aqueous solution of hydroxides of the alkali metal and ammonium or amine; and (d) contacting the aqueous hydroxide solution of the alkali metal and ammonia or amine with a cation exchange resin at conditions sufficient to selectively remove essentially all the alkali metal from the liquid.
Claim 12
Dependent Claim
55 words
The method of claim 9 wherein the condensate is contacted with a resin bed comprising a mixture of an anion exchange resin and a cation exchange resin and the mixed resin bed is separated into an anion resin rich layer and a caton resin rich layer prior to the regeneration of the cation exchange resin.
Claim 13
Dependent Claim
40 words
The method of claim 10 wherein the anion and cation exchange resins are separated in the presence of an inert interfacial material which forms a layer positioned between the layer of cation resin and layer of anion resin upon separation.
Claim 14
Dependent Claim
45 words
The method of claim 10 wherein the cation exchange resin in alkaline earth metal form is regenerated by converting any nonmagnesium alkaline earth metal cations on the cation resin with magnesium cations and subsequently contacting the magnesium form of the cation resin with sulfuric acid.
Claim 15
Dependent Claim
79 words
The method of claim 10 wherein the exchange of the alkali earth metal and ammonium or amine cations on the strong acid cation resin with alkaline earth metal cations is conducted by contacting the resin with at least about 1.1 times the stoichiometrically equivalent amount of an aqueous solution of calcium hydroxide being from about 0.1 to about 0.4 Normal, said stoichiometric amount being based on the equivalents of alkali metal and ammonium or amine cations on the resin.
Claim 16
Dependent Claim
94 words
The method of claim 13 wherein, following the exchange of the alkali metal and ammonium or amine cations with the calcium cations, the strong acid cation resin in calcium form is contacted with an amount of an aqueous salt solution of magnesium which comprises from about 0.1 to about 20 weight percent of the magnesium salt based on the weight of the magnesium salt, said amount comprising at least about 1.2 times the stoichiometrically equivalent amount of the calcium cations on the strong acid cation resin, and the resin in magnesium form subsequently regenerated.
Claim 17
Dependent Claim
22 words
The method of claim 14 wherein the regeneration of the cation resin in magnesium form comprises contacting the resin with sulfuric acid.
Claim 18
Dependent Claim
15 words
The method of claim 10 wherein the ammonia or amine is recycled to the condensate.
Claim 19
Dependent Claim
28 words
The method of claim 10 wherein the regenerated anion and cation exchange resins are reused in purifying the condensate containing the alkali metal and ammonium or amine cations.
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) | 1984-04-20 | 1984-10-20 | 1985-04-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-04-20 | 1988-10-20 | 1989-04-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-04-20 | 1992-10-20 | 1993-04-21 | $7700.00 | Window Closed / Lapsed |