US4424144A
Expired / Lapsed
US
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Preparation of binderless 3A adsorbents
Assignee: WR Grace and Co Conn
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Filing: 1981-11-16
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Granted: 1984-01-03
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Expires: 2001-11-16
Abstract
Abstract Shaped products of a 3A zeolite are formed either as beads or extrudates without any binder remaining. In the case of beads, a 4A powder is mixed with a caustic solution and a metakaolin clay binder to form beads. The beads are converted to a binderless 4A product which is given a partial calcium exchange followed by a potassium exchange to obtain the desired 3A binderless bead. The 3A extrudates are produced by forming binderless 4A extrudates from a 4A powder and clay mixture that contains 40-60% by weight clay. These binderless 4A extrudates are then given a potassium exchange. Both the beads and the extrudates can be used to dry a mixture of a hydrocarbon compound such as ethylene and water.
Inventors
- 👤 James N. Pryor
- 👤 Chang W. Chi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 14:51
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815; C01B33/283; B; B01; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; B01J20/183; C07; C07C; C07C7/00; C07C7/12; C07C7/13; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/52; Y02P30/00; Y02P30/40; Y10; Y10S; Y10S423/00; Y10S423/24
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
111 words
A process of making 3A zeolite binderless beads comprising forming beads from a mixture of 4A zeolite powder, a clay binder and a sodium hydroxide solution; treating the beads with additional sodium hydroxide to convert the clay binder to a 4A zeolite to provide a 4A binderless bead; partially exchanging the 4A binderless bead with a calcium containing solution to form an intermediate bead product; exchanging the intermediate bead product with a potassium exchanging solution selected from the group consisting of an aqueous solution of a potassium salt, a potassium hydroxide solution and mixtures thereof to obtain a 3A zeolite binderless bead; and recovering and activating the potassium exchanged bead product.
Claim 2
Dependent Claim
111 words
A process of making 3A zeolite binderless beads comprising forming beads from a mixture of 4A zeolite powder, a clay binder and a sodium hydroxide solution; treating the beads with additional sodium hydroxide to convert the clay binder to a 4A zeolite to provide a 4A binderless bead; partially exchanging the 4A binderless bead with a calcium containing solution to form an intermediate bead product; exchanging the intermediate bead product with a potassium exchanging solution selected from the group consisting of an aqueous solution of a potassium salt, a potassium hydroxide solution and mixtures thereof to obtain a 3A zeolite binderless bead; and recovering and activating the potassium exchanged bead product.
Claim 3
Dependent Claim
25 words
The process according to claim 1, wherein the recovering and activating step comprises washing the potassium exchanged beads, drying and calcining to remove adsorbed water.
Claim 4
Dependent Claim
18 words
The process according to claim 1, wherein the potassium exchange solution is an aqueous solution of potassium chloride.
Claim 5
Dependent Claim
33 words
The process according to claim 1, wherein the partial calcium exchange is carried out so that the intermediate bead product has a calcium content, measured as CaO, of about 2.0 -3.0 wt. %.
Claim 6
Dependent Claim
13 words
The process according to claim 1, wherein the clay is a metakaolin clay.
Claim 7
Dependent Claim
12 words
The adsorbent 3A binderless bead made by the process of claim 1.
Claim 8
Dependent Claim
146 words
A process for making a binderless 3A extrudate from an extrudable mixture of a synthetic 4A zeolite, metakaolin clay, and sodium hydroxide solution, said clay comprising about 40-60% by weight of the total weight of the clay and the zeolite on a dry basis and the amount of sodium hydroxide being in the range of about 90-120% of the stoichiometric amount to convert the clay to a zeolite, said process comprising extruding the extrudable mixture to form extrudates; aging the extrudates; treating the aged extrudates with a dilute solution of sodium hydroxide at an elevated temperature to complete the crystallization of the aged extrudates; washing the crystallized extrudates; contacting the washed extrudates with a potassium exchanging solution selected from the group consisting of an aqueous solution of a potassium salt, a potassium hydroxide solution and mixtures thereof; and recovering and activating the potassium exchanged extrudate product.
Claim 9
Dependent Claim
146 words
A process for making a binderless 3A extrudate from an extrudable mixture of a synthetic 4A zeolite, metakaolin clay, and sodium hydroxide solution, said clay comprising about 40-60% by weight of the total weight of the clay and the zeolite on a dry basis and the amount of sodium hydroxide being in the range of about 90-120% of the stoichiometric amount to convert the clay to a zeolite, said process comprising extruding the extrudable mixture to form extrudates; aging the extrudates; treating the aged extrudates with a dilute solution of sodium hydroxide at an elevated temperature to complete the crystallization of the aged extrudates; washing the crystallized extrudates; contacting the washed extrudates with a potassium exchanging solution selected from the group consisting of an aqueous solution of a potassium salt, a potassium hydroxide solution and mixtures thereof; and recovering and activating the potassium exchanged extrudate product.
Claim 10
Dependent Claim
25 words
The process according to claim 7, wherein the recovering and activating step comprises washing the potassium exchanged beads, drying and calcining to remove adsorbed water.
Claim 11
Dependent Claim
18 words
The process according to claim 7, wherein the potassium exchange solution is an aqueous solution of potassium chloride.
Claim 12
Dependent Claim
12 words
The adsorbent 3A binderless extrudate made by the process of claim 7.
Claim 13
Dependent Claim
40 words
A 3A binderless bead adsorbent made from a mixture of metakaolin clay and a synthetic 4A zeolite where the clay is present from about 40-60% by weight on a dry basis of the total weight of the clay and zeolite.
Claim 14
Dependent Claim
40 words
A 3A binderless bead adsorbent made from a mixture of metakaolin clay and a synthetic 4A zeolite where the clay is present from about 40-60% by weight on a dry basis of the total weight of the clay and zeolite.
Claim 15
Dependent Claim
40 words
A 3A binderless extrudate adsorbent made from a mixture of metakaolin clay and a synthetic 4A zeolite where the clay is present from about 40-60% by weight on a dry basis of the total weight of the clay and zeolite.
Claim 16
Dependent Claim
40 words
A 3A binderless extrudate adsorbent made from a mixture of metakaolin clay and a synthetic 4A zeolite where the clay is present from about 40-60% by weight on a dry basis of the total weight of the clay and zeolite.
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) | 1987-01-02 | 1987-07-04 | 1988-01-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-01-02 | 1991-07-04 | 1992-01-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-01-02 | 1995-07-04 | 1996-01-03 | $7700.00 | Window Closed / Lapsed |