CA2367798A1 - Polymer-cement composites and methods of making same - Google Patents
Polymer-cement composites and methods of making same Download PDFInfo
- Publication number
- CA2367798A1 CA2367798A1 CA 2367798 CA2367798A CA2367798A1 CA 2367798 A1 CA2367798 A1 CA 2367798A1 CA 2367798 CA2367798 CA 2367798 CA 2367798 A CA2367798 A CA 2367798A CA 2367798 A1 CA2367798 A1 CA 2367798A1
- Authority
- CA
- Canada
- Prior art keywords
- polymer
- cement
- cement composite
- silica
- latex
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract 38
- 239000011414 polymer cement Substances 0.000 title claims abstract 37
- 238000000034 method Methods 0.000 title claims 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract 59
- 239000000377 silicon dioxide Substances 0.000 claims abstract 26
- 239000004568 cement Substances 0.000 claims abstract 15
- 239000004816 latex Substances 0.000 claims abstract 15
- 229920000126 latex Polymers 0.000 claims abstract 15
- 239000000463 material Substances 0.000 claims abstract 9
- 239000007787 solid Substances 0.000 claims abstract 9
- 239000002245 particle Substances 0.000 claims abstract 8
- 239000004576 sand Substances 0.000 claims abstract 7
- 239000011256 inorganic filler Substances 0.000 claims abstract 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract 6
- 239000011398 Portland cement Substances 0.000 claims abstract 5
- 239000007900 aqueous suspension Substances 0.000 claims abstract 5
- 239000007788 liquid Substances 0.000 claims abstract 5
- 239000000203 mixture Substances 0.000 claims abstract 5
- 239000011396 hydraulic cement Substances 0.000 claims abstract 4
- 238000007580 dry-mixing Methods 0.000 claims abstract 3
- 238000002156 mixing Methods 0.000 claims abstract 3
- 229920000642 polymer Polymers 0.000 claims 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 9
- 239000000654 additive Substances 0.000 claims 4
- 238000001035 drying Methods 0.000 claims 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- 239000010881 fly ash Substances 0.000 claims 3
- 239000000725 suspension Substances 0.000 claims 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims 2
- 239000000292 calcium oxide Substances 0.000 claims 2
- 235000012255 calcium oxide Nutrition 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000000465 moulding Methods 0.000 claims 2
- 239000000049 pigment Substances 0.000 claims 2
- 229920000058 polyacrylate Polymers 0.000 claims 2
- 238000003825 pressing Methods 0.000 claims 2
- 230000003014 reinforcing effect Effects 0.000 claims 2
- 150000003839 salts Chemical class 0.000 claims 2
- 229910021487 silica fume Inorganic materials 0.000 claims 2
- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 claims 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical class C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims 1
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000002174 Styrene-butadiene Substances 0.000 claims 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims 1
- 238000005266 casting Methods 0.000 claims 1
- 238000009750 centrifugal casting Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 claims 1
- 239000010459 dolomite Substances 0.000 claims 1
- 229910000514 dolomite Inorganic materials 0.000 claims 1
- 239000004744 fabric Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- 239000000945 filler Substances 0.000 claims 1
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical class O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 claims 1
- 239000010434 nepheline Substances 0.000 claims 1
- 229910052664 nepheline Inorganic materials 0.000 claims 1
- 239000010451 perlite Substances 0.000 claims 1
- 235000019362 perlite Nutrition 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- 239000002893 slag Substances 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 239000011115 styrene butadiene Substances 0.000 claims 1
- 229920003048 styrene butadiene rubber Polymers 0.000 claims 1
- 239000010435 syenite Substances 0.000 claims 1
- 229920001169 thermoplastic Polymers 0.000 claims 1
- 239000010455 vermiculite Substances 0.000 claims 1
- 229910052902 vermiculite Inorganic materials 0.000 claims 1
- 235000019354 vermiculite Nutrition 0.000 claims 1
- 229920003169 water-soluble polymer Polymers 0.000 claims 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
Abstract
A polymer-cement composite comprises, by weight percent, about 40% to 50%
inert, inorganic filler material, such as silica sand; about 12% to 23% latex, preferably in aqueous suspension; about 20% to 25% hydraulic cement; and about 6% to 14%
reactive silica. The reactive silica is a pozzolanic material, and in preferred embodiments, where the cement is portland cement, comprises an advantageous mixture of precipitated and ground silica. All solid components have a particle size of less than about 300 microns.
The polymer-cement composite is preferably made by dry mixing of the powdered components throughly in a high intensity mixer, adding the liquid components, and wet mixing to form a thoroughly blended, de-aired green mixture. The green mixture is formed into any desired shape, cured, and dried. Preferably, the product is cured in a warm, moist environment.
inert, inorganic filler material, such as silica sand; about 12% to 23% latex, preferably in aqueous suspension; about 20% to 25% hydraulic cement; and about 6% to 14%
reactive silica. The reactive silica is a pozzolanic material, and in preferred embodiments, where the cement is portland cement, comprises an advantageous mixture of precipitated and ground silica. All solid components have a particle size of less than about 300 microns.
The polymer-cement composite is preferably made by dry mixing of the powdered components throughly in a high intensity mixer, adding the liquid components, and wet mixing to form a thoroughly blended, de-aired green mixture. The green mixture is formed into any desired shape, cured, and dried. Preferably, the product is cured in a warm, moist environment.
Claims (45)
1. A polymer-cement composite comprising:
inert, inorganic filler material;
latex;
cement;
reactive silica;
optional additives; and water.
inert, inorganic filler material;
latex;
cement;
reactive silica;
optional additives; and water.
2. The polymer-cement composite of claim 1 wherein the composite comprises, by weight percent, about 40 % to 50 % inert, inorganic filler material;
about 12 % to 23 % latex; about 20 % to 25 % cement; about 7 % to 13 %
reactive silica; and the remainder being optional additives and water.
about 12 % to 23 % latex; about 20 % to 25 % cement; about 7 % to 13 %
reactive silica; and the remainder being optional additives and water.
3. The polymer-cement composite of claim 1 wherein all solid components have particle sizes less than 300 microns.
4. The polymer-cement composite of claim 1 wherein the reactive silica is a pozzolanic material.
5. The polymer-cement composite of claim 1 wherein the inert, inorganic filler material is selected from the group consisting of silica sand, ground nepheline syenite, ground sandstone, ground limestone, ground dolomite, coarse fly ash, and ground basalt.
6. The polymer-cement composite of claim 5 wherein the inert, inorganic filler is silica sand.
7. The polymer-cement composite of claim 6 wherein the silica sand has a particle size ranging from about 50 to 300 microns.
8. The polymer-cement composite of claim 1 wherein the inert, inorganic filler is a lightweight, fine aggregate material.
9. The polymer-cement composite of claim 8 wherein the lightweight, fine aggregate material is selected from the group consisting of fly ash, perlite, and vermiculite.
10. The polymer-cement composite of claim 1 wherein the polymer solids in the latex are redispersible.
11. The polymer-cement composite of claim 1 wherein the polymer solids in the latex are in an aqueous suspension.
12. The polymer-cement composite of claim 11 wherein the latex is a colloidal suspension of polymer in water containing about 50 percent by weight of spherical polymer particles ranging in size from about 0.01 micron to 1 micron in diameter.
13. The polymer-cement composite of claim 12 wherein the colloidal suspension comprises about 56-58 percent by weight latex solids.
14. The polymer-cement composite of claim 1 wherein the polymer solids of the latex are selected from the group consisting of elastomeric polymers;
thermoplastic polymers; and alkali-swellable latexes.
thermoplastic polymers; and alkali-swellable latexes.
15. The polymer-cement composite of claim 14 wherein the latex is an aqueous suspension of polyacrylate polymer.
16. The polymer-cement composite of claim 14 wherein the latex is an aqueous suspension of styrene-butadiene polymer.
17. The polymer-cement composite of claim 14 wherein the latex is an aqueous suspension of styrene-acrylate polymer.
18. The polymer-cement composite of claim 1 wherein the cement is an hydraulic cement.
19. The polymer-cement composite of claim 18 wherein the hydraulic cement is selected from the group consisting of portland cement and calcium aluminate cements.
20. The polymer-cement composite of claim 19 wherein the hydraulic cement is portland cement having a particle size range from about 1 to 100 microns, with median particle sizes in the 10 to 15 micron range.
21. The polymer-cement composite of claim 1 wherein the reactive silica is selected from the group consisting of ground silica, silica fume (microsilica), precipitated silica, fly ash, and ground blast furnace slag or mixtures thereof.
22. The polymer-cement composite of claim 21 wherein the reactive silica has an average particle size range from about 0.01 to 45 microns.
23. The polymer-cement composite of claim 1 wherein the components are present in the following ratios:
Components Ratio 1 water/cement 0.43-0.49 by weight 2 water/(cement+reactive 0.30-0.34 by weight silica) 3 latex solids/cement 0.30-0.60 by weight 4 filler/cement 1.90-2.10 by weight reactive silica/cement 0.28-0.61 by weight 6 calcia/total reactive silica 0.80-1.30 by moles
Components Ratio 1 water/cement 0.43-0.49 by weight 2 water/(cement+reactive 0.30-0.34 by weight silica) 3 latex solids/cement 0.30-0.60 by weight 4 filler/cement 1.90-2.10 by weight reactive silica/cement 0.28-0.61 by weight 6 calcia/total reactive silica 0.80-1.30 by moles
24. The polymer-cement composite of claim 1 wherein the optional additives are selected from the group consisting of pigments and admixtures.
25. The polymer-cement composite of claim 24 wherein the admixture is an organic, water-soluble polymer useful for plasticizing.
26. The polymer-cement composite of claim 25 wherein the admixtures is selected from the group consisting of salts of sulphonated napthalene formaldehyde polymers and salts of sulphonated melamine formaldehyde polymers.
27. The polymer-cement composite of claim 1 further comprising reinforcing means.
28. The polymer-cement composite of claim 27 wherein the reinforcing means are selected from the group consisting of discrete or continuous fibers and steel cloth, mesh, or rods.
29. A polymer-cement composite comprising:
silica sand;
latex;
portland cement;
a mixture of ground silica and precipitated silica;
water; and optionally, additives.
silica sand;
latex;
portland cement;
a mixture of ground silica and precipitated silica;
water; and optionally, additives.
30. The polymer-cement composite of claim 29 comprising:
Material Avg. Particle Size Range of Addition 1 Silica Sand 130 µm 41-48 wt%
2 Latex: Suspension -- 13-22 wt %
(Solids) 0.2 µm (7-13 wt% ) 3 Portland Cement 10-15 µm 20-25 wt%
4 Ground Silica 3.7 µm 5-12 wt%
5 Precipitated Silica 0.015 µm 1-2 wt%
6 Pigments 0.1-1.0 µm 0-1 wt%
7 Admixtures -- 0-2 wt %
8 Water -- 0-5 wt %
Material Avg. Particle Size Range of Addition 1 Silica Sand 130 µm 41-48 wt%
2 Latex: Suspension -- 13-22 wt %
(Solids) 0.2 µm (7-13 wt% ) 3 Portland Cement 10-15 µm 20-25 wt%
4 Ground Silica 3.7 µm 5-12 wt%
5 Precipitated Silica 0.015 µm 1-2 wt%
6 Pigments 0.1-1.0 µm 0-1 wt%
7 Admixtures -- 0-2 wt %
8 Water -- 0-5 wt %
31. The polymer-cement composite of claim 30 wherein the components are present in the following ratios:
Components Ratio 1 water/cement 0.43-0.49 by weight 2 water/(cement+ reactive 0.30-0.34 by weight silica) 3 latex solids/cement 0.30-0.60 by weight 4 sand/cement 1.90-2.10 by weight reactive silica/cement 0.28-0.61 by weight 6 calcia/total reactive silica 0.80-1.30 by moles
Components Ratio 1 water/cement 0.43-0.49 by weight 2 water/(cement+ reactive 0.30-0.34 by weight silica) 3 latex solids/cement 0.30-0.60 by weight 4 sand/cement 1.90-2.10 by weight reactive silica/cement 0.28-0.61 by weight 6 calcia/total reactive silica 0.80-1.30 by moles
32. A method of making a polymer-cement composite comprising the steps of:
(a) dry mixing the powdered components;
(b) adding the liquid components;
(c) wet mixing of the powdered and liquid components to form the green body;
(d) forming the green body into the desired shape of a product;
(e) curing the product; and (f) drying the product.
(a) dry mixing the powdered components;
(b) adding the liquid components;
(c) wet mixing of the powdered and liquid components to form the green body;
(d) forming the green body into the desired shape of a product;
(e) curing the product; and (f) drying the product.
33. A method of making a polymer-cement composite comprising the steps of:
(a) dry mixing the powdered components of the polymer-cement composite in a high intensity mixer until homogeneous;
(b) adding the liquid components under vacuum; and (c) wet mixing the powdered and liquid components at medium intensity to form a thououghly mixed batch of green body which is de-aired.
(a) dry mixing the powdered components of the polymer-cement composite in a high intensity mixer until homogeneous;
(b) adding the liquid components under vacuum; and (c) wet mixing the powdered and liquid components at medium intensity to form a thououghly mixed batch of green body which is de-aired.
34. The method of claim 33 comprising the further step(s) of:
(d) forming the mixed batch into the desired shape.
(d) forming the mixed batch into the desired shape.
35. The method of claim 34 wherein the step of forming the mixed batch into the desired shape is selected from the group consisting of any of the following methods: extruding, molding, pressing, vibratory casting, and centrifugal casting.
36. The method of claim 34 wherein the step of forming the mixed batch into the desired shape comprises:
vacuum extruding flat sheets from the mixed batch;
cutting the extruded sheets to the desired size;
placing the sheets into molds;
pressing the sheets in the molds to shape; and de-molding the product.
vacuum extruding flat sheets from the mixed batch;
cutting the extruded sheets to the desired size;
placing the sheets into molds;
pressing the sheets in the molds to shape; and de-molding the product.
37. The method of claim 33 including the further step of:
curing .
curing .
38. The method of claim 37 wherein the step of curing is conducted in a moist environment.
39. The method of claim 38 wherein the step of curing in a moist environment comprises:
curing in high pressure, saturated steam in an autoclave.
curing in high pressure, saturated steam in an autoclave.
40. The method of claim 39 wherein the step of curing in an autoclave comprises slowly heating the product at a maximum rate of about 60 ° C
to 80 ° C
per hour to a temperature in the range of about 125 ° to 180 ° C
for about 2 to 12 hours.
to 80 ° C
per hour to a temperature in the range of about 125 ° to 180 ° C
for about 2 to 12 hours.
41. The method of claim 38 wherein the step of curing in a moist environment comprises:
warm, moist curing.
warm, moist curing.
42. The method of claim 41 wherein step of warm, moist curing comprises curing in a moist environment having a relative humidity ranging from about 85 % to 95 % at a temperature of about 45 °C to 55 °C for about 6 to 14 days.
43. The method of claim 37 comprising the further step of, prior to curing, pre-curing at a room temperature in a moist environment having from about 85 % to 95 % relative humidity for up to 1 day.
44. The method of claim 37 comprising the further step of drying the product.
45. The method of claim 44 wherein the step of drying comprises the steps of:
heating the product to about 85° C at a rate of about 15 ° C per hour and holding the product at temperature for about 16 to 24 hours; and final drying the product by increasing the temperature to about 105°C, at a rate of about 15°C per hour, and holding the product at temperature for about 24 hours .
heating the product to about 85° C at a rate of about 15 ° C per hour and holding the product at temperature for about 16 to 24 hours; and final drying the product by increasing the temperature to about 105°C, at a rate of about 15°C per hour, and holding the product at temperature for about 24 hours .
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12532799P | 1999-03-19 | 1999-03-19 | |
| US60/125,327 | 1999-03-19 | ||
| PCT/US2000/007192 WO2000056679A1 (en) | 1999-03-19 | 2000-03-17 | Polymer-cement composites and methods of making same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2367798A1 true CA2367798A1 (en) | 2000-09-28 |
| CA2367798C CA2367798C (en) | 2010-10-19 |
Family
ID=22419223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 2367798 Expired - Fee Related CA2367798C (en) | 1999-03-19 | 2000-03-17 | Polymer-cement composites and methods of making same |
Country Status (9)
| Country | Link |
|---|---|
| US (2) | US6569923B1 (en) |
| EP (1) | EP1187794B1 (en) |
| JP (1) | JP2002540050A (en) |
| AT (1) | ATE361265T1 (en) |
| AU (1) | AU3897700A (en) |
| CA (1) | CA2367798C (en) |
| DE (1) | DE60034674T2 (en) |
| MX (1) | MXPA01009447A (en) |
| WO (1) | WO2000056679A1 (en) |
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| US20080015104A1 (en) * | 2006-07-13 | 2008-01-17 | Unimin Corporation | Ultrafine nepheline syenite |
| US20080040980A1 (en) * | 2006-07-13 | 2008-02-21 | Unimin Corporation | Method of processing nepheline syenite |
| US8858699B2 (en) | 2006-07-13 | 2014-10-14 | Unimin Corporation | Ultra fine nepheline syenite powder and products for using same |
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| US9302448B2 (en) * | 2006-08-23 | 2016-04-05 | United States Gypsum Company | Flexible cementitious membrane composite and associated crack-isolation floor systems |
| ITPN20060064A1 (en) * | 2006-08-24 | 2008-02-25 | Sergio Fregonese | CEMENTITIOUS COMPOSITION OF INSULATING MATERIALS OF VARIOUS KIND |
| NL1032501C2 (en) * | 2006-09-14 | 2008-03-17 | Rudolf Van Hardeveld | Method for the production of ceramic filter materials for the capture of (ultra) fine particles from a gas or liquid stream. |
| US7757976B2 (en) * | 2007-02-07 | 2010-07-20 | Unimin Corporation | Method of processing nepheline syenite powder to produce an ultra-fine grain size product |
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| US11384029B2 (en) | 2019-03-18 | 2022-07-12 | The Regents Of The University Of California | Formulations and processing of cementitious components to meet target strength and CO2 uptake criteria |
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| US6569923B1 (en) | 2003-05-27 |
| DE60034674D1 (en) | 2007-06-14 |
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| DE60034674T2 (en) | 2008-01-17 |
| MXPA01009447A (en) | 2003-08-19 |
| US8017672B2 (en) | 2011-09-13 |
| AU3897700A (en) | 2000-10-09 |
| ATE361265T1 (en) | 2007-05-15 |
| WO2000056679A1 (en) | 2000-09-28 |
| EP1187794B1 (en) | 2007-05-02 |
| CA2367798C (en) | 2010-10-19 |
| EP1187794A1 (en) | 2002-03-20 |
| US20040204516A1 (en) | 2004-10-14 |
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