An additive for, a method of adding thereof to uncured mixes for and resulting cured cement-type concreations such as cured embodiments of concrete, marcadam, and roof-top shingles each exhibiting improved heat and freeze-thaw durability resulting from reduced efflorescence and stability against sun ultraviolet light exposure.

Patent
   RE37655
Priority
Sep 12 1997
Filed
Aug 19 2000
Issued
Apr 16 2002
Expiry
Sep 12 2017
Assg.orig
Entity
Large
3
35
all paid
1. An anti efflorescence cementitious additive comprising in combination chemically different compounds "a)" and "b)", compound "a)" including at least one particulated polymer having particles sizes of about 0.01 angstroms to about 10,000 angstroms, and compound "b)" including at-least one hydrophobic compound, said particulated polymer ranging in weight from about 5 percent to about 75 percent by combined weights of the particulated polymer and the hydrophobic component.
87. A cementitious additive composition for reducing efflorescence and improving durability of cementitious composition comprising (a) about 5 to about 75 weight percent of at least one particulate polymer compound selected from the group consisting of polyepoxide, styrene butadiene, polyvinyl acetate, acrylonitrile-butadiene latex rubber, polyacrylic ester, polyvinylidene chloride-vinyl chloride, polyethylene-vinyl acetate, acrylic latex,. calcium stearate, ethylene-vinyl acetate, polyacrylic ester, polyurethane, and acrylic latex, and (b) at least one hydrophobic compound, wherein the particulated polymer has a size ranging from about 0.01 angstroms to about 10,000 angstroms.
2. The additive of claim 1, wherein said particulated polymer ranges in weight from about 25 percent to about 50 percent of combined compounds "a)" and "b)".
3. The additive of claim 2, wherein said particulated polymer comprises polyepoxide in a major amount, and in which said particles range in size from about 0.05 angstroms to about 1500 angstroms.
4. The additive of claim 2, in which said particulated polymer comprises styrene butadiene.
5. The additive of claim 2, in which said particulated polymer comprises polyvinylacetate.
6. The additive of claim 2, in which said particulated polymer comprises acrylonitrile-butadiene rubber.
7. The additive of claim 2, in which said particulated polymer comprises polyacrylic ester.
8. The additive of claim 2, in which said particulated polymer comprises polyvinylidene.
9. The additive of claim 2, in which said particulated polymer comprises chloride-vinyl chloride.
10. The additive of claim 2, in which said particulated polymer comprises polyethylene-vinyl acetate.
11. The additive of claim 2, in which said particulated polymer comprises polyepoxide.
12. The additive of claim 2, in which said particulated polymer comprises polyurethane.
13. The additive of claim 2, in which said particulated polymer comprises acrylic latex.
14. The additive of claim 2, in which said particulated polymer comprises calcium stearate.
15. The additive of claim 2, in which said particulated polymer comprises additionally a copolymer.
16. The additive of claim 15, in which said particulated polymer additionally comprises polyvinyl acetate.
17. The additive of claim 15, in which said particulated polymer additionally comprises polyethylene-vinyl acetate.
18. The additive of claim 1, in which said particulated polymer comprises styrene butadiene.
19. The additive of claim 1, in which said particulated polymer comprises polyvinyl acetate.
20. The additive of claim 1, in which said particulated polymer comprises acrylonitrile-butadiene rubber.
21. The additive of claim 1, in which said particulated polymer comprises polyacrylic ester.
22. The additive of claim 1, in which said particulated polymer comprises polyvinylidene.
23. The additive of claim 1, in which said particulated polymer comprises chloride-vinyl chloride.
24. The additive of claim 1, in which said particulated polymer comprises polyethylene-vinyl acetate.
25. The additive of claim 1, in which said particulated polymer comprises polyepoxide.
26. The additive of claim 1, in which said particulated polymer comprises polyurethane.
27. The additive of claim 1, in which said particulated polymer comprises acrylic latex.
28. The additive of claim 1, in which said particulated polymer comprises calcium stearate.
29. The additive of claim 1, further comprising a stone substrate.
30. The additive of claim 29, in which said stone substrate comprises sand as a predominate and major portion thereof.
31. The additive of claim 30, further comprising oil in an amount sufficient to impart water-barrier properties and improved durability against repetitious heat and thaw temperature changes.
32. The additive of claim 29, in which said stone substrate comprises concrete pavement.
33. The additive of claim 29, in which said stone substrate component comprises crushed stone of sizes substantially larger than sand, as a predominate and major portion thereof.
34. The additive of claim 33, further comprising a tar binder.
35. The additive of claim 34, in which said tar binder comprises at least a major proportion of a naturally-occuring tar.
36. The additive of claim 34, in which said tar binder comprises at least a major proportion of a synthetic tar.
37. An article comprising the additive of claim 29, and paper layers adhered together by a tar binder.
38. A ready-mix anti-efflorescence composition comprising the additive of claim 34 and marcadam macadam in a tar-set state.
39. A ready-mix anti-efflorescence composition comprising the additive of claim 34 and a cementitious ingredient in a water-set state.
40. A ready-mix anti-efflorescence composition comprising the additive of claim 30 and a cementitious ingredient in a water-set state.
41. A method of making the additive of claim 1, comprising admixing said compound b) with said compound a).
42. The additive of claim 1, in which said compound b) comprises a blend of calcium stearate, zinc stearate, and aluminum stearate.
43. The additive of claim 42, wherein said blend further comprises at least one of a dispersant, a plasticizer, a lubricant, a salt scavenger, or a viscosity modifier.
44. The additive of claim 1, in which said at least one particulated polymer comprises a polymer blend of styrene butadiene, polyepoxide, and acrylonitrile-butadiene latex-rubber and is present in an amount sufficient to impart improved durability.
45. The additive of claim 43, in which said lubricant comprises an effective lubricating amount of cocomide diethyl amine.
46. The additive of claim 43, in which said plasticizer comprises an effective plasticizing amount of lignon sulfonate.
47. The additive of claim 43, in which said dispersant comprises an effective dispersing amount of sodium polyacrylate.
48. The additive of claim 43, in which said salt scavanger scavenger comprises an effective salt-scavenging amount of barium carbonate.
49. The additive of claim 43, in which said viscosity modifier comprises an effective viscosity-modifying amount of carageenan pre-blended in ethylene glycol.
50. The additive of claim 44, further comprising an effective amount of a biological-control agent.
51. An anti-efflorescence cementitious composition comprising a cementitious material and the additive of claim 1, in which said particulated polymer comprises polyurethane and is present in an effective amount sufficient to impart improved durability against degradation.
52. The additive of claim 1, additionally including: 1) a stone substrate comprising sand as a predominate and major portion thereof; 2) a dispersant; 3) a plasticizer, 4) a lubricant, 5) a salt scavenger, and 6) a viscosity modifier.
53. The additive of claim 3, additionally including: 1) a stone substrate comprising sand as a predominate and major portion thereof; 2) a dispersant; 3) a plasticizer, 4) a lubricant, 5) a salt scavenger, and 6) a viscosity modifier.
54. The additive of claim 44, additionally including: 1) a stone substrate comprising sand as a predominate and major portion thereof; 2) a dispersant; 3) a plasticizer, 4) a lubricant, 5) a salt scavenger, and 6) a viscosity modifier.
55. A method of making the additive of claim 43, comprising in combination, the steps of:
1) first-admixing compound b), a lubricant, a salt scavenger, and a viscosity modifier, the first-admixing including critically maintaining temperature of the admixture within a range of from about 50 degrees Fahrenheit to about 200 degrees Fahrenheit, to form a first admixture; and
2) second-admixing compound a) with said first admixture, to form a second admixture, said second-admixing including intermittently adding and blending small increment-amounts of said compound a) to said first admixture, wherein the additive contains compound a) in an amount of about 5 to about 95 weight percent of said first admixture.
56. The method of claim 55, in which said temperature is maintained within a range of from about 95 degrees Fahrenheit to about 120 degrees Fahrenheit during admixing and blending.
57. The method of claim 56, in which said amount of component a) ranges from about 50% to about 75% by weight of said first admixture.
58. The method of claim 55, in which said amount of component a) ranges from about 50% to about 75% by weight of said first admixture.
59. The method of claim 56, in which said compound a) comprises a polymer blend of styrene butadiene, polyepoxide, and acrylonitrile-butadiene latex-rubber and is present in amounts sufficient for the blend to imart impart improved durability against heat and thaw deterioration.
60. The method of claim 57, in which said compound a) comprises a polymer blend of styrene butadiene, polyepoxide, and acrylonitrile-butadiene latex-rubber, each polymer of the blend being present in amounts sufficient for the polymer blend to impart improved durability against heat and thaw deterioration.
61. The method of claim 57, in which said compound a) comprises a polymer blend of styrene butadiene, polyepoxide, and acrylonitrile-butadiene latex-rubber, and is present in an amount sufficient for the polymer blend to impart improved durability against repetitious heat and thaw conditions.
62. An anti-efflorescence composition comprising (1) the additive of claim 1, (2) a particulated stone substrate, and (3) at-least one of particulated alumina, lime, iron oxide or magnesia.
63. A method of making a cementitious composition, comprising in combination, the steps of sufficiently admixing the additive of claim 1 with a particulated cement in an amount sufficient for the additive composition to be present in an amount between about 2 percent and about 20 percent on a weight percentage basis.
64. A method of making a cement composition comprising in combination, the steps of sufficiently admixing the additive of claim 3 with a particulated cement in an amount sufficient for the additive composition to be present in an amount between about 2 percent and about 20 percent on a weight percentage basis.
65. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polycarbonate.
66. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyester.
67. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polymethylmethacrylate.
68. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyoxyethylidene.
69. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyethylene.
70. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polypropylene.
71. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polystyrene.
72. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyurethane.
73. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyepoxide.
74. The anti-efflorescence additive of claim 2, in which said particulated polymer comprises polyvinylacetate.
75. The anti-efflorescence additive of claim 1, in which said compound a) is durable at temperatures within a range of from about 75 degrees Fahrenheit to about 800 degrees Fahrenheit.
76. The anti-efflorescence additive of claim 74, in which said compound a) is alkaline-stable.
77. The anti-efflorescence additive of claim 1, in which said compound a) is insoluble in a media having a pH including and ranging from neutral through acidic.
78. The additive of claim 2, in which said particulated polymer comprises polyterephthalate.
79. The anti-efflorescence additive of claim 78, in which said compound a) is insoluble in media having a pH including and ranging from neutral through acidic.
80. The anti-efflorescence additive of claim 76, in which said compound a) is substantially stable against degredation degradation when exposed to ultraviolet exposure ranging upwardly through at-least 100 cycles of a D65 light source of a weatherometer.
81. The anti-efflorescence additive of claim 1, in which said compound a) is substantially stable against degredation degradation when exposed to ultraviolet exposure ranging upwardly through at-least 100 cycles of a D65 light source of a weatherometer.
82. The anti-efflorescence additive of claim 79 77, in which said particulated polymer ranges in weight from about 25 percent to about 50 percent, and in which said particles range in size within a range of from about 0.05 angstroms to about 1500 angstroms.
83. The anti-efflorescence additive of claim 79 77, in which said compound(s) b) range(s) in weight from about 5 percent to about 75 percent by weight of total anti-efflorescence additive.
84. The anti-efflorescence additive of claim 79 77, wherein said compound(s) b) is present in an amount ranging in weight from about 25 percent to about 50 percent by weight of total anti-efflorescence additive.
85. The additive of claim 53, in which said compound(s) b) range(s) in weight from about 1 percent to about 40 percent by weight of total additive.
86. The additive of claim 53, in which said compound(s) b) range(s) in weight from about 5 percent to about 10 percent by weight of total additive.
88. The additive of claim 87, wherein the polymer comprises polyepoxide having a size of about 0.05 angstroms to about 1500 angstroms.
89. The additive of claim 87, further comprising sand.
90. The additive of claim 1, further comprising oil in an amount sufficient to impart water-barrier properties to the additive.
91. A method of making the additive composition of claim 87, comprising admixing compound a) and compound b).
92. The additive according to claim 87, wherein the hydrophobic compound comprises a blend of calcium stearate, zinc stearate and aluminum stearate.
93. The additive according to claim 92, wherein the hydrophobic blend further comprises at least one of a dispersant, a plasticizer, a lubricant, a salt scavenger and a viscosity modifier.
94. A cementitious composition comprising cement and the additive according to claim 87, and further comprising sand, a dispersant, a plasticizer, a lubricant, a salt scavenger and a viscosity modifier.

Prior art patents include U.S. Pat. No. 3,645,763 issued Feb. 29, 1972 to Anathony R. Ronzio et. al., U.S. Pat. No. 3,895,953 issued Jul. 22, 1975 to Povindar K. Mehta et al., U.S. Pat. No. 4,268,316 issued May 19, 1981 to Milton H. Wills, Jr., U.S. Pat. No. 4,434,193 issued Feb. 28, 1984 to Thomas Beckenhauer, U.S. Pat. No. 4,983,220 issued Jan. 8, 1991 to Alain Mathieu, U.S. Pat. No. 4,999,218 issued Mar. 12, 1991 to Gerd Rebner, et al., U.S. Pat. No. 5,460,648 issued Oct. 24, 1995 to Craig T. Walloch et al., U.S. Pat. No. 5,494,741 issued Feb. 27, 1996 to Frank Fekete, U.S. Pat. No. 5,531,824 issued Jul. 2, 1996 to J. Pate Burkes et al., U.S. Pat. No. 5,595,594 issued Jul. 21, 1997 to Jier-Yi Dong et al.

In the relevant trade heretofore up to the time of the present invention, it became apparent to those skilled in the art that preexisting cured cements,

Typically and preferably a vessel is water jacketed for cooling and has dimensions such that the height is about 2.5 times greater than the width or diameter of the rotor stator assembly. The rotor stator employed is preferably a variable-speed, center offset and top-mounted with preferably adjustable height capability. Rotor speed is adjusted as appropriate for adequate mixing together with holding it down sufficiently to prevent vortexing and/or air entrainment. Thereafter typically (but not limited to) about 1% by weight of the prior admixed formulation, are added of each of lubricant (such as typically Cocomide Diethyl amine), dispersant (such as sodium polyacrylate), salt scavenger (such as barium carbonate), and concurrently or thereafter blended for about fifteen minutes (more of less as might be required for reasonable substantially homogeneous admixing thereof). Thereafter a preblended viscosity modifier such as typically Carageenan extract, preblended at about 15% by weight of the total preblend weight, with typically ethylene glycol, is substantially slowly added to the extent required for thorough and complete mixing, to the prior mix, followed by agitation-admixing thereof for typically about ten minutes more or less. Preferably thereafter, there is added any desired or conventional biological control agent in a conventional amount of typically about 0.3 percent by weight of the total prior foregoing admixture, followed by continued or additional admixing for a period of typically about five minutes. Thereafter, the particulated polymer or blend of two or more thereof, is thereupon blended/admixed with the prior aforenoted mix. Typically and preferably there are employed a blend of particulated polymer of styrene butadiene at about 75 percent of the blend weight, about 5 percent of poly epoxy, and about 20 percent of acrylic latex, typically admixed/prepared at normal low speed marine type agitator blending, at a rotor speed drastically reduced (held low) sufficiently to give a blending capacity only to the system. Thereafter sufficient polymer or polymer blend is added (preferably gradually)to the foregoing prepared admixture, such that the finished polymer admixture contains about 35 percent of the aforenoted first-prepared admixture, and about 65 percent more or less, of the added polymer or polymer blend. During addition and following thorough admixture, the admixing period is for about 15 minutes or longer as might be required for substantially homogeneous admixing thereof. At aforenoted percentages, the particulated polymer or blend of polymers is/are present in amounts broadly ranging from about 5 percent to 95 percent, but normally and preferably typically from about 50 percent to about 75 percent, based on the weight of the entire resulting total composition-mix.

This invention is premised on the discovery that efflorescence control agents can be designed with the desired performance characteristics in a particular system, by altering the chemical composition of the ECA with a performance driven polymer blend. This polymer blend allows for improved polymer particle to cement (for example) particle interaction. The polymer and/or blend of a plurality thereof, of the polymers of this invention, may be engineered for application to a plurality of different specific applications. For example, a styrene butadiene component lends both stability and durability against repeated freeze-freeze-thaw and/or elevated temperature exposures. For example, epoxy component provides especially preferred additional strength characteristics to the final cured cement-type concreations. Likewise, acrylic latex provides especially improved stability against ultra violet radiation repeated exposures as well providing enhance non-yellowing durability and/or stability of the cured cement-type concreations.

While not bound to any given theory as to the reasons why nor specific mechanism resulting in the aforenoted improvements and/or advantages of this invention, it has become apparent that more that one instance of synergism exists as previously stated. Additionally however, it has become clear and conclusive that critically the particle size of the particulated polymer(s), together with the aforestated broad and preferred weight ranges, results in the achievement of the objects of the present invention, within the particle broad and more preferred ranges above-stated. Apart therefrom, within the particular polymer(s)-hydrophobic combination(s), there are additionally the aforenoted preferred embodiments each of which obtain further maximized beneficial results characterized by aforenoted objects. Also, through extensive experimentation and testing, it became apparent that the present invention extends over a broad spectrum of cement-type concreations and methods of preparation thereof. For example, apart from aforestated preferred embodiments of cured ultimate products, one thereof is directed to concrete roof tile(s) utilized in warmer or hot climates, where excessive heat exposures is the primary problem--thus requiring the additive blend to be modified slightly to be directed more specifically at that problem--not being faced with heat-freeze-thaw cycles; in such warmer environment(s), there is also typically greater exposure to ultraviolet light and to excessive amounts of rain, each and/or both requiring conventional modifications in the formula to meet the primary problems of that/those climatic and/or geographical area(s).

A plurality of various probative tests were employed by the inventor, in testing for the presence or absence of aforenoted problems with control(s) and various blends of the composition(s) of the present invention.

This example is directed to a composition and procedure relating to durability of a concrete segmental retaining wall unit.

To a laboratory batching kitchen aid mixer, 150 grams, of normal type 1 cement was added. In addition, 1350 grams of stone and sand fitted to any optimized aggregate blend curve for a typical retaining wall with an FM of 3.70 was added. In addition, a red iron oxide pigment was added at 3.0% based on the weight of cement (4.5 grams). The cement, aggregate and pigment were blended for two minutes. Sixty grams of water was added sufficient to attain a water to cement ratio of 0.40. The material was then blended for an additional 90 seconds. At that point, 2.45 grams (25 ounces per hundred weight of cement equivalent) of the efflorescence control agent and polymer blend were added to the mix. The efflorescence control agent(s) (ECA) represents 35% by weight and the polymer blend represents 65% by weight. The ECA was a modified calcium stearate. The polymer blend in this instance is 75% styrene butadiene, 20% ultraviolet (UV) stabilized acrylic latex, and 5% polyepoxy. The sample was mixed for an additional 90 second and then 375 grams of the mix was placed in a steel paver mold and pressed with a hydraulic press to 2000 psi. This sample procedure is repeated a total of four times. The entire procedure is repeated in a control having no admixture and a sample containing a pure calcium stearate ECA. An additional sample is generated using a 20% cement content and a standard non-ionic detergent plasticizer at 4 fluid ounces per hundred weight of cement equivalent. The samples are cured at 135 degrees Fahrenheit and 95% relative humidity for 16 hours. At 28 days the samples are then subjected to durability testing according to ASTM 1262 in both fresh water and saline. The samples are also subjected to weatherometer testing for accelerated efflorescence formation determination and are rated at 100 cycles. The samples are rated on a scale ranging from zero (0) to 5.0, the "0" being "no efflorescence" and "5" being complete surface coverage with deposits; the data is displayed in the FIG. I. FIG. 2 represents the effects for each of those categories in varying percentages thereof versus # of cycles of freezefreeze-thaw via ASTM C1262 Saline Testing inventive polymer blend/ECA combination exhibiting marked superior excellent freeze/freeze-thaw durability. FIG. 3 illustrates the fresh water testing/ASTM C1262 Fresh Water Testing, and represents the effects for each of those categories in varying percentages thereof versus # of cycles of freeze-freeze-thaw. The inventive polymer blend/ECA combination continued to exhibit marked superior excellent freeze-thaw durability.

For the same categories as aforenoted example, comparing compressive strength (as psi) versus different temperatures in a series of different comparisons, FIG. 4 likewise exhibits marked superior performances as regards compressive strength for each comparison. FIG. 5 likewise exhibits marked superior performance in permeability, as regards centimeter(s) (cm) per hour for each comparison.

For the same categories as aforenoted Example 1, but here on a full scale basis for a production series of units manufactured in an Allen Block Segmental Retaining Wall style, the illustrated results of FIGS. 6, 7 and 8 confirm tests comparable to Example 1 and FIGS. 1 through 3, confirming marked superiority in all categories.

For the same categories as aforenoted Example 1 (and foregoing FIGS. 1 through 3), identical tests of Example 4 as illustrated in FIGS. 9 through 11 comparing permeability coefficient (cm/psi) versus different temperatures in a series of different comparisons, FIG. IV for concrete pavingstone likewise exhibits marked superior performance of the additive and concrete pavingstone embodiment.

For the embodiment of concrete rooftile utilizing 1125 grams of solely sand as aggregate, utilizing (3% by weight of cement) 11.25 grams, and differing from Example 1, adding 150 grams of water, after mixing, followed by adding 150 grams of water (water-cement ratio of 0.40). The thereafter 2.50 grams of ECA added represents 35% by weight and 65% by weight of the polymer-ECA mix thereof. After the sample thereafter was mixed for an additional 90 seconds, 375 grams of the mix is placed in a steel block mold and pressed with a hydraulic press to 1000 psi. This sample procedure was repeated a total of 4 times. The entire procedure was repeated in a control having no admixture and likewise there was prepared a sample containing a pure calcium stearate ECA. An additional sample was generated using no integral admixture but applying a surface acrylic latex surface sealer to both a wet and fully cured series of samples. Otherwise, this procedure was the same as that of Example 1. For the same categories as aforenoted examples, as illustrated here in FIGS. 12 through 14, the inventive combination likewise again exhibits marked superior performance in all categories.

For the same categories as aforenoted examples, Example 6 for an embodiment of concrete masonry unit, utilizing the same stone and sand aggregate as Example 1, the procedure and amounts were the same as for preceding Example 1. Utilizing the same tests as for Example 1, the results reflected in corresponding FIGS. 15 through 17 likewise exhibits marked superior performance for the present invention in all categories.

For the same categories as aforenoted examples, in testing a ready mix concrete or pressed concrete material, the cement added was the normal type 1, and the iron oxide pigment added was black iron oxide still at 3.0% based on the weight of cement; and after the blending thereof, water was added at 100 grams of water, at the same water-to-cement ratio of 0.40. The thereafter added efflorescence control agent (ECA) was 2.50 grams (25 ounces per hundred weight of cement) was employed--representing 35% by weight and the polymer blend represents 65%. The polymer blend included 60% styrene butadiene, 25 UV stabilized acrylic latex, and 15% polyepoxy. The sample was mixed for an additional 90 seconds and then 375 grams of the mix was placed into a steel mold and given a quick trowel finish. This procedure was repeated a total of four times. The entire procedure was repeated in a control having no admixture, and thereafter again in an additional sample containing a pure calcium stearate ECA. An additional sample was generated using a momomericially available calcium stearate based water resistance admixture. The samples were cured at room temperature and humidity overnight. At 28 days the samples were then subjected to testing as in Example 1. Otherwise, the procedure hereinabove corresponded to (the same as that of) Example 1. The tests as illustrated in FIGS. 18 through 20, for all categories tested, likewise exhibited marked superior performance for the present invention, as regards centimeter(s) (cm) per hour for each comparison.

Supplee, William W.

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