Patent US4076618A successfully refreshed from Google Patents.
US4076618A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Treatment of liquids containing complexed heavy metals and complexing agents
Assignee: AMP Akzo Corp
•
Filing: 1976-07-09
•
Granted: 1978-02-28
•
Expires: 1996-07-09
Abstract
Abstract Methods are provided for separating by-products from alkanolamine complexing agents and heavy metals complexed with alkanolamines, and for the waste-treating of solutions containing such complexed heavy metals and complexing agents. Illustratively, the pH of an electroless metal deposition bath or bath effluent which contains an alkanolamine complexing agent and an alkanolamine-complexed heavy metal is adjusted to render the complexing agent and complexed heavy metal extractable by an ion exchange medium, the pH-adjusted bath liquid is contacted with an ion-exchange medium capable of extracting the complexed heavy metal and complexing agent, the contacted bath liquid, which contains by-products and is substantially free of the complexed heavy metal and the complexing agent is removed from the ion exchange medium and the complexed heavy metal and complexing agent are recovered from the exchange medium for further use in electroless metal deposition baths.
Inventors
- 👤 Rudolph J. Zeblisky
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 22:50
CPC Classifications
B; B01; B01J; B01J45/00; C; C22; C22B; C22B3/00; C22B3/20; C22B3/26; C22B3/28; C22B3/286; C22B3/42; C23; C23C; C23C18/00; C23C18/16; C23C18/1601; C23C18/1617; Y; Y02; Y02P; Y02P10/00; Y02P10/20; Y10; Y10S; Y10S210/00; Y10S210/902; Y10S210/911; Y10S210/912
Claims Analysis
Total Claims: 38
Claim 1
Independent Claim
170 words
A method of separating alkali metal salt by-products of an electroless metal deposition bath from an alkanolamine complexing agent and a complex species of a heavy metal complexed with an alkanolamine complexing agent in an alkaline electroless metal deposition bath, said method comprising : a. lowering the pH of said alkaline bath or alkaline effluent thereof to render said alkanolamine complexed heavy metal and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. removing from the exchange medium a bath liquid which comprises said alkali metal salt by-products and which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; d. removing said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the exchange medium, and e. returning said alkanolamine-complexed heavy metal and said alkanolamine complexing agent to an alkaline electroless metal deposition bath.
Claim 2
Independent Claim
170 words
A method of separating alkali metal salt by-products of an electroless metal deposition bath from an alkanolamine complexing agent and a complex species of a heavy metal complexed with an alkanolamine complexing agent in an alkaline electroless metal deposition bath, said method comprising : a. lowering the pH of said alkaline bath or alkaline effluent thereof to render said alkanolamine complexed heavy metal and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. removing from the exchange medium a bath liquid which comprises said alkali metal salt by-products and which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; d. removing said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the exchange medium, and e. returning said alkanolamine-complexed heavy metal and said alkanolamine complexing agent to an alkaline electroless metal deposition bath.
Claim 3
Dependent Claim
30 words
A method as defined in claim 1 wherein before step (a), the pH of the electroless metal deposition bath is in the range of from about 11 to about 13.5.
Claim 4
Dependent Claim
22 words
A method as defined in claim 1 wherein in step (a), the pH is lowered to a value of less than 11.
Claim 5
Dependent Claim
28 words
A method as defined in claim 3 wherein in step (a), the pH is lowered to a value in the range of from about 3 to about 7.5.
Claim 6
Dependent Claim
31 words
A method as defined in claim 1 wherein the alkanolamine complexing agent is selected from the group consisting of N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine, triethanolamine, ethylenedinitrilotetraethanol, nitrilotri-2-propanol, tetrahydroxyethylethylenediamine, monohydroxyethyl-trihydroxypropyl-ethylenediamine or mixtures thereof.
Claim 7
Dependent Claim
16 words
A method as defined in claim 5 wherein the complexing agent is N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine.
Claim 8
Dependent Claim
24 words
A method as defined in claim 1 wherein the heavy metal is selected from the group consisting of copper, nickel, cobalt, and alloys thereof.
Claim 9
Dependent Claim
30 words
A method as defined in claim 1 wherein the ion exchange medium is selected from the group consisting of cation exchange resins and ion exchange resins having a chelating functionality.
Claim 10
Dependent Claim
22 words
A method as defined in claim 8 wherein said cation exchange resin comprises a polystyrene resin having --SO 3 - ionic groups.
Claim 11
Dependent Claim
32 words
A method as defined in claim 1 wherein the pH-adjusted bath liquid is sequentially contacted in step (b) with a cation exchange resin and an ion exchange resin having a chelating functionality.
Claim 12
Dependent Claim
27 words
A method as defined in claim 1 wherein the specific gravity of the bath or bath effluent prior to treatment in step (a)is no greater than 1.075.
Claim 13
Dependent Claim
29 words
A method as defined in claim 1 wherein in step (d), said complexed heavy metal and said complexing agent are removed from the exchange medium by an alkaline solution.
Claim 14
Dependent Claim
34 words
A method as defined in claim 1 wherein in step (d), said complexed heavy metal and said complexing agent are removed from the exchange medium by an electroless metal deposition bath or effluent therefrom.
Claim 15
Independent Claim
181 words
A method of separating alkali metal salt by-products of an electroless copper deposition bath from an alkanolamine complexing agent and a complex species of copper complexed with an alkanolamine complexing agent in an alkaline electroless copper deposition bath, said method comprising: a. lowering the pH of said alkaline bath or alkaline effluent thereof to less than 11, to render said alkanolamine-complexed copper and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed copper and said alkanolamine complexing agent from the pH-adjusted bath liquid, said ion exchange medium being selected from the group consisting of cation exchange resins and chelating exchange resins; c. removing from said exchange medium a bath liquid comprises alkali metal salt by-products and which is substantially free of said alkanolamine-complexed copper and said alkanolamine complexing agent; d. removing said alkanolamine-complexed copper and said alkanolamine complexing agent from the exchange medium, and e. returning said alkanolamine-complexed copper and said alkanolamine complexing agent to an alkaline electroless metal deposition bath.
Claim 16
Independent Claim
181 words
A method of separating alkali metal salt by-products of an electroless copper deposition bath from an alkanolamine complexing agent and a complex species of copper complexed with an alkanolamine complexing agent in an alkaline electroless copper deposition bath, said method comprising: a. lowering the pH of said alkaline bath or alkaline effluent thereof to less than 11, to render said alkanolamine-complexed copper and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed copper and said alkanolamine complexing agent from the pH-adjusted bath liquid, said ion exchange medium being selected from the group consisting of cation exchange resins and chelating exchange resins; c. removing from said exchange medium a bath liquid comprises alkali metal salt by-products and which is substantially free of said alkanolamine-complexed copper and said alkanolamine complexing agent; d. removing said alkanolamine-complexed copper and said alkanolamine complexing agent from the exchange medium, and e. returning said alkanolamine-complexed copper and said alkanolamine complexing agent to an alkaline electroless metal deposition bath.
Claim 17
Independent Claim
151 words
A method of separating alkali metal salt by-products of an electroless metal deposition bath from an alkanolamine complexing agent and a complex species of a heavy metal complexed with an alkanolamine complexing agent in an alkaline electroless metal deposition bath, said method comprising: a. lowering the pH of said alkaline bath or alkaline effluent thereof to render said alkanolamine complexed heavy metal and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. removing from the exchange medium a bath liquid which comprises said alkali metal salt by-products and which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; and d. removing said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the exchange medium.
Claim 18
Independent Claim
151 words
A method of separating alkali metal salt by-products of an electroless metal deposition bath from an alkanolamine complexing agent and a complex species of a heavy metal complexed with an alkanolamine complexing agent in an alkaline electroless metal deposition bath, said method comprising: a. lowering the pH of said alkaline bath or alkaline effluent thereof to render said alkanolamine complexed heavy metal and said alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjusted bath liquid of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. removing from the exchange medium a bath liquid which comprises said alkali metal salt by-products and which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; and d. removing said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the exchange medium.
Claim 19
Dependent Claim
30 words
A method as defined in claim 15 wherein before step (a), the pH of the electroless metal deposition bath is in the range of from about 11 to about 13.5.
Claim 20
Dependent Claim
22 words
A method as defined in claim 15 wherein in step (a), the pH is lowered to a value of less than 11.
Claim 21
Dependent Claim
28 words
A method as defined in claim 17 wherein in step (a), the pH is lowered to a value in the range of from about 3 to about 7.5.
Claim 22
Dependent Claim
31 words
A method as defined in claim 15 wherein the alkanolamine complexing agent is selected from the group consisting of N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine, triethanolamine, ethylenedinitrilotetraethanol, nitrilo-tri-2-propanol, tetrahydroxyethylethylenediamine, monohydroxyethyl-trihydroxypropyl-ethylenediamine or mixtures thereof.
Claim 23
Dependent Claim
16 words
A method as defined in claim 19 wherein the complexing agent is N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine.
Claim 24
Dependent Claim
24 words
A method as defined in claim 15 wherein the heavy metal is selected from the group consisting of copper, nickel, cobalt, and alloys thereof.
Claim 25
Dependent Claim
30 words
A method as defined in claim 15 wherein the ion exchange medium is selected from the group consisting of cation exchange resins and ion exchange resins having a chelating functionality.
Claim 26
Dependent Claim
22 words
A method as defined in claim 22 wherein said cation exchange resin comprises a polystyrene resin having --SO 3 - ionic groups.
Claim 27
Dependent Claim
32 words
A method as defined in claim 15 wherein the pH-adjusted bath liquid is sequentially contacted in step (b) with a cation exchange resin and an ion exchange resin having a chelating functionality.
Claim 28
Dependent Claim
28 words
A method as defined in claim 15 wherein the specific gravity of the bath or bath effluent prior to treatment in step (a) is no greater than 1.075.
Claim 29
Dependent Claim
25 words
A method as defined in claim 15 wherein said complexed heavy metal and complexing agent are removed from the exchange medium by an alkaline solution.
Claim 30
Independent Claim
111 words
A method of treating an aqueous alkaline solution comprising an alkanolamine complexing agent and a heavy metal complexed with an alkanolamine complexing agent, said method comprising: a. lowering the pH of said alkaline solution to render the alkanolamine-complexed heavy metal and the alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjust solution of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. discharging from the ion exchange medium a liquid which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; an d. regenerating the ion exchange medium.
Claim 31
Independent Claim
111 words
A method of treating an aqueous alkaline solution comprising an alkanolamine complexing agent and a heavy metal complexed with an alkanolamine complexing agent, said method comprising: a. lowering the pH of said alkaline solution to render the alkanolamine-complexed heavy metal and the alkanolamine complexing agent extractable by an ion exchange medium; b. contacting the pH-adjust solution of step (a) with an ion exchange medium capable of extracting said alkanolamine-complexed heavy metal and said alkanolamine complexing agent from the pH-adjusted bath liquid; c. discharging from the ion exchange medium a liquid which is substantially free of said alkanolamine-complexed heavy metal and said alkanolamine complexing agent; an d. regenerating the ion exchange medium.
Claim 32
Dependent Claim
22 words
A method as defined in claim 27 wherein in step (a), the pH is lowered to a value of less than 11.
Claim 33
Dependent Claim
28 words
A method as defined in claim 28 wherein in step (a), the pH is lowered to a value in the range of from about 3 to about 7.5.
Claim 34
Dependent Claim
31 words
A method as defined in claim 27 wherein the alkanolamine complexing agent is selected from the group consisting of N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine, triethanolamine, ethylenedinitrilotetraethanol, nitrilotri-2-propanol, tetrahydroxyethylethylenediamine, monohydroxyethyl-trihydroxypropyl-ethylenediamine or mixures thereof.
Claim 35
Dependent Claim
16 words
A method as defined in claim 30 wherein the complexing agent is N, N, N', N'-tetrakis-(2-hydroxypropyl)-ethylenediamine.
Claim 36
Dependent Claim
24 words
A method as defined in claim 27 wherein the heavy metal is selected from the group consisting of copper, nickel, cobalt, and alloys thereof.
Claim 37
Dependent Claim
30 words
A method as defined in claim 27 wherein the ion exchange medium is selected from the group consisting of cation exchange resins and ion exchange resins having a chelating functionality.
Claim 38
Dependent Claim
32 words
A method as defined in claim 27 wherein the pH-adjusted bath liquid is sequentially contacted in step (b) with a cation exchange resin and an ion exchange resin having a chelating functionality.
References Cited (Backward Citations)
US3148947A
Cited
US3119709A
Cited
US3075855A
Cited
US3003866A
Cited
US3558288A
Cited
US3658470A
Cited
US3882018A
Cited
US3998627A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-02-27 | 1981-08-29 | 1982-02-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-02-27 | 1985-08-29 | 1986-02-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-02-27 | 1989-08-29 | 1990-02-28 | $7700.00 | Window Closed / Lapsed |