Patent US5470813A successfully refreshed from Google Patents.
US5470813A
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Double metal cyanide complex catalysts
Assignee: Lyondell Chemical Technology LP
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Filing: 1993-11-23
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Granted: 1995-11-28
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Expires: 2013-11-23
Abstract
Abstract Improved double metal cyanide catalysts are disclosed. The substantially amorphous catalysts of the invention are more active for polymerizing epoxides than conventional DMC catalysts, which have a substantial crystalline component. Polyol products made with the catalysts are unusually clear, have exceptionally low unsaturations, and contain no detectable amount of low molecular weight polyol impurities. A method of making the improved DMC catalysts, which involves intimately combining the reactants, is also disclosed.
Inventors
- 👤 Bi Le-Khac
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 18:42
CPC Classifications
C; C08; C08G; C08G65/00; C08G65/02; C08G65/26; C08G65/2642; C08G65/2645; C08G65/2663; B; B01; B01J; B01J27/00; B01J27/24; B01J27/26; C08G59/00; C08G59/18; C08G65/30
Claims Analysis
Total Claims: 45
Claim 1
Independent Claim
27 words
A catalyst which comprises at least about 70 wt. % of a substantially amorphous double metal cyanide (DMC) complex, wherein the catalyst is useful for polymerizing epoxides.
Claim 2
Dependent Claim
27 words
A catalyst which comprises at least about 70 wt. % of a substantially amorphous double metal cyanide (DMC) complex, wherein the catalyst is useful for polymerizing epoxides.
Claim 3
Dependent Claim
19 words
The catalyst of claim 1 which comprises at least about 90 wt. % of the substantially amorphous DMC complex.
Claim 4
Dependent Claim
19 words
The catalyst of claim 1 which comprises at least about 99 wt. % of the substantially amorphous DMC complex.
Claim 5
Dependent Claim
13 words
The catalyst of claim 1 wherein the DMC complex is a zinc hexacyanocobaltate.
Claim 6
Dependent Claim
13 words
The catalyst of claim 4 prepared using tert-butyl alcohol as a complexing agent.
Claim 7
Dependent Claim
41 words
A composition which comprises at least about 70 wt. % of a substantially amorphous DMC complex catalyst, and up to about 30 wt. % of a highly crystalline DMC compound, wherein the composition is useful as a catalyst for polymerizing epoxides.
Claim 8
Dependent Claim
41 words
A composition which comprises at least about 70 wt. % of a substantially amorphous DMC complex catalyst, and up to about 30 wt. % of a highly crystalline DMC compound, wherein the composition is useful as a catalyst for polymerizing epoxides.
Claim 9
Dependent Claim
33 words
The composition of claim 6 which comprises at least about 90 wt. % of the substantially amorphous DMC complex catalyst, and up to about 10 wt. % of the highly crystalline DMC compound.
Claim 10
Dependent Claim
33 words
The composition of claim 6 which comprises at least about 99 wt. % of the substantially amorphous DMC complex catalyst, and up to about 1 wt. % of the highly crystalline DMC compound.
Claim 11
Dependent Claim
17 words
A catalyst which consists essentially of a substantially amorphous double metal cyanide complex useful for polymerizing epoxides.
Claim 12
Dependent Claim
17 words
A catalyst which consists essentially of a substantially amorphous double metal cyanide complex useful for polymerizing epoxides.
Claim 13
Dependent Claim
19 words
The catalyst of claim 9 which contains less than about 1 wt. % of a highly crystalline DMC compound.
Claim 14
Dependent Claim
16 words
The catalyst of claim 9 having a surface area less than about 30 m 2 /g.
Claim 15
Dependent Claim
13 words
The catalyst of claim 9 wherein the DMC complex is a zinc hexacyanocobaltate.
Claim 16
Dependent Claim
13 words
The catalyst of claim 12 prepared using tert-butyl alcohol as a complexing agent.
Claim 17
Independent Claim
59 words
A method of making a double metal cyanide (DMC) complex catalyst, said method comprising: (a) intimately combining and reacting aqueous solutions of a water-soluble metal salt and a water-soluble metal cyanide salt in the presence of a complexing agent to produce an aqueous mixture containing a precipitated DMC complex catalyst; and (b) isolating and drying the DMC complex catalyst.
Claim 18
Independent Claim
59 words
A method of making a double metal cyanide (DMC) complex catalyst, said method comprising: (a) intimately combining and reacting aqueous solutions of a water-soluble metal salt and a water-soluble metal cyanide salt in the presence of a complexing agent to produce an aqueous mixture containing a precipitated DMC complex catalyst; and (b) isolating and drying the DMC complex catalyst.
Claim 19
Dependent Claim
23 words
The method of claim 14 wherein the resulting catalyst further comprises up to about 30 wt. % of a highly crystalline DMC compound.
Claim 20
Dependent Claim
20 words
The method of claim 14 wherein the resulting catalyst has a surface area less than about 30 m 2 /g.
Claim 21
Dependent Claim
17 words
The method of claim 14 wherein the aqueous salt solutions are intimately combined by a homogenization process.
Claim 22
Dependent Claim
28 words
The method of claim 14 wherein the complexing agent is selected from the group consisting of alcohols, aldehydes, ketones, ethers, esters, amides, ureas, nitriles, sulfides, and mixtures thereof.
Claim 23
Dependent Claim
34 words
The method of claim 14 wherein the complexing agent is a water-soluble aliphatic alcohol selected from the group consisting of ethanol, isopropyl alcohol, n-butyl alcohol, sec-butyl alcohol, tert-butyl alcohol, isobutyl alcohol, and mixtures thereof.
Claim 24
Dependent Claim
38 words
The method of claim 14 wherein the resulting catalyst prepared by intimately combining the reactants is at least about 65% more active as an epoxide polymerization catalyst than a similar catalyst prepared by simple mixing of the reactants.
Claim 25
Dependent Claim
38 words
The method of claim 14 wherein the resulting catalyst prepared by intimately combining the reactants is at least about 200% more active as an epoxide polymerization catalyst than a similar catalyst prepared by simple mixing of the reactants.
Claim 26
Dependent Claim
11 words
A DMC complex catalyst made by the method of claim 14.
Claim 27
Dependent Claim
45 words
A catalyst which consists essentially of a substantially amorphous zinc hexacyanocobaltate complex, wherein the catalyst is prepared in the presence of a water-soluble aliphatic alcohol complexing agent selected from the group consisting of ethanol, isopropyl alcohol, tert-butyl alcohol, sec-butyl alcohol, n-butyl alcohol, and isobutyl alcohol.
Claim 28
Dependent Claim
45 words
A catalyst which consists essentially of a substantially amorphous zinc hexacyanocobaltate complex, wherein the catalyst is prepared in the presence of a water-soluble aliphatic alcohol complexing agent selected from the group consisting of ethanol, isopropyl alcohol, tert-butyl alcohol, sec-butyl alcohol, n-butyl alcohol, and isobutyl alcohol.
Claim 29
Dependent Claim
37 words
The catalyst of claim 23 which exhibits an X-ray diffraction pattern of (d-spacing, angstroms): 4.82 (br), 3.76 (br), and exhibits no detectable signals corresponding to highly crystalline zinc hexacyanocobaltate at about (d-spacing, angstroms): 5.07, 3.59, 2.54, 2.28.
Claim 30
Dependent Claim
17 words
A double metal cyanide complex catalyst having a surface area less than about 30 m 2 /g.
Claim 31
Dependent Claim
17 words
A double metal cyanide complex catalyst having a surface area less than about 30 m 2 /g.
Claim 32
Dependent Claim
16 words
The catalyst of claim 25 having a surface area less than about 20 m 2 /g.
Claim 33
Dependent Claim
54 words
A double metal cyanide catalyst which is the reaction product of a water-soluble metal salt, a water-soluble metal cyanide salt, and a complexing agent, wherein the catalyst is effective to polymerize propylene oxide at a rate in excess of 3 g PO/min/100 ppm catalyst, based on the weight of finished polyether, at 105° C.
Claim 34
Dependent Claim
54 words
A double metal cyanide catalyst which is the reaction product of a water-soluble metal salt, a water-soluble metal cyanide salt, and a complexing agent, wherein the catalyst is effective to polymerize propylene oxide at a rate in excess of 3 g PO/min/100 ppm catalyst, based on the weight of finished polyether, at 105° C.
Claim 35
Dependent Claim
54 words
A double metal cyanide catalyst which is the reaction product of a water-soluble metal salt, a water-soluble metal cyanide salt, and a complexing agent, wherein the catalyst is effective to polymerize propylene oxide at a rate in excess of 5 g PO/min/250 ppm catalyst, based on the weight of finished polyether, at 105° C.
Claim 36
Dependent Claim
54 words
A double metal cyanide catalyst which is the reaction product of a water-soluble metal salt, a water-soluble metal cyanide salt, and a complexing agent, wherein the catalyst is effective to polymerize propylene oxide at a rate in excess of 5 g PO/min/250 ppm catalyst, based on the weight of finished polyether, at 105° C.
Claim 37
Dependent Claim
27 words
The catalyst of claim 1 wherein the substantially amorphous DMC complex exhibits a powder x-ray diffraction pattern having substantially no sharp lines at about 5.1 (d-spacing, angstroms).
Claim 38
Dependent Claim
25 words
The method of claim 14 wherein the resulting catalyst exhibits a powder x-ray diffraction pattern having substantially no sharp lines at about 5.1 (d-spacing, angstroms).
Claim 39
Dependent Claim
28 words
The catalyst of claim 23 wherein the substantially amorphous zinc hexacyanocobaltate complex exhibits a powder x-ray diffraction pattern having substantially no sharp lines at about 5.1 (d-spacing, angstroms).
Claim 40
Dependent Claim
24 words
A double metal cyanide (DMC) complex catalyst that exhibits a powder x-ray diffraction pattern having substantially no sharp lines at about 5.1 (d-spacing, angstroms).
Claim 41
Dependent Claim
24 words
A double metal cyanide (DMC) complex catalyst that exhibits a powder x-ray diffraction pattern having substantially no sharp lines at about 5.1 (d-spacing, angstroms).
Claim 42
Dependent Claim
17 words
A DMC catalyst which comprises at least about 70 wt. % of the catalyst of claim 32.
Claim 43
Dependent Claim
16 words
The catalyst of claim 32 having a surface area less than about 30 m 2 /g.
Claim 44
Dependent Claim
45 words
The method of claim 20 wherein the DMC complex catalyst is a zinc hexacyanocobaltate, and the activity of the catalyst is measured for the polymerization of propylene oxide at 105° C. using a catalyst level of 100 ppm based on the weight of finished polyol.
Claim 45
Dependent Claim
42 words
The method of claim 21 wherein the DMC complex catalyst is a zinc hexacyanocobaltate, and the activity of the catalyst is measured for the polymerization of propylene oxide at 105° C. using a catalyst level of 250 ppm in the finished polyol.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1998-11-27 | 1999-05-29 | 1999-11-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2002-11-27 | 2003-05-29 | 2003-11-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2006-11-27 | 2007-05-29 | 2007-11-28 | $7700.00 | Window Closed / Lapsed |