US4664820A — Preactivated organophilic clay gellant lubricatin…

Claim 1

Independent Claim 123 words

A dry preactivated organophilic clay gellant for lubricating greases comprising: (a) an organophilic clay gellant which is the reaction product of (i) a smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay, and (ii) organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type clay; and (b) a preactivating agent reacted with the organophilic clay gellant, said preactivating agent being from about 1 to about 25% by weight of the organophilic clay gellant and being selected from the group consisting of phthalide, 3-hydroxy-4-methoxy benzaldehyde, 4-benzyloxypropiophenone, triethyl citrate, 2-phenoxyethanol, 1-phenyl-1,2-ethanediol, o-, m- and p-nitrobenzyl alcohol, 1,6-hexanediol, castor oil, o-, m- and p-nitrophenethyl alcohol, and mixtures thereof.

Claim 2

Dependent Claim 123 words

A dry preactivated organophilic clay gellant for lubricating greases comprising: (a) an organophilic clay gellant which is the reaction product of (i) a smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay, and (ii) organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type clay; and (b) a preactivating agent reacted with the organophilic clay gellant, said preactivating agent being from about 1 to about 25% by weight of the organophilic clay gellant and being selected from the group consisting of phthalide, 3-hydroxy-4-methoxy benzaldehyde, 4-benzyloxypropiophenone, triethyl citrate, 2-phenoxyethanol, 1-phenyl-1,2-ethanediol, o-, m- and p-nitrobenzyl alcohol, 1,6-hexanediol, castor oil, o-, m- and p-nitrophenethyl alcohol, and mixtures thereof.

Claim 3

Dependent Claim 25 words

The dry preactivated organophilic clay gellant of claim 1 wherein the smectite-type clay is selected from the group consisting of bentonite, hectorite, and mixtures thereof.

Claim 4

Dependent Claim 15 words

The dry preactivated organophilic clay gellant of claim 2 wherein the smectite-type clay is bentonite.

Claim 5

Dependent Claim 31 words

The dry preactivated organophilic clay gellant of claim 1 wherein the amount of organic cation is from about 100 to about 130% of the cation exchange capacity of the smectite-type clay.

Claim 6

Dependent Claim 30 words

The dry preactivated organophilic clay gellant of claim 4 wherein the amount of organic cation is from about 100 to about 116% of the cation exchange capacity of smectite-type clay.

Claim 7

Dependent Claim 31 words

The dry preactivated organophilic clay gellant of claim 1 wherein the organic cation contains at least one lineal or branched, saturated or unsaturated alkyl group having 12 to 22 carbon atoms.

Claim 8

Dependent Claim 139 words

The dry preactivated organophilic clay gellant of claim 6 wherein the organic cation is at least one of ##STR4## wherein X is a nitrogen or phosphorous, Y is sulfur, R 1 is a lineal or branched, saturated or unsaturated alkyl group having 12 to 22 carbon atoms and R 2 , R 3 and R 4 are independently selected from (a) lineal or branched alkyl groups having 1 to 22 carbon atoms; (b) aralkyl group which are benzyl and substituted benzyl moieties including fused ring moieties having lineal or branched 1 to 22 carbon atoms in the alkyl portion of the structure: (c) aryl groups such as phenyl and substituted phenyl including fused ring aromatic substituents; (d) beta, gamma- unsaturated groups having six or less carbon atoms or hydroxylalkyl groups having 2 to 6 carbon atoms; and (e) hydrogen.

Claim 9

Dependent Claim 56 words

The dry preactivated organophilic clay gellant of claim 7 wherein the organic cation is ammonium, R 1 and R 2 are lineal or branched, saturated or unsaturated alkyl groups having 12 to 22 carbon atoms and R 3 and R 4 are lineal or branched, saturated or unsaturated alkyl groups having 1 to 12 carbon atoms.

Claim 10

Dependent Claim 18 words

The dry preactivated organophilic clay gellant of claim 8 wherein the organic cation is dimethyl bis(hydrogenated tallow) ammonium.

Claim 11

Dependent Claim 61 words

The dry preactivated organophilic clay gellant of claim 7 wherein the organic cation is ammonium, R 2 is an aralkyl group having a lineal or branched, saturated or unsaturated alkyl group having 1 to 12 carbons in the alkyl portion and R 3 and R 4 are lineal or branched, saturated or unsaturated alkyl groups having 1 to 12 carbon atoms.

Claim 12

Dependent Claim 19 words

The dry preactivated organophilic clay gellant of claim 10 wherein the organic cation is dimethyl benzyl hydrogenated tallow ammonium.

Claim 13

Dependent Claim 27 words

The dry preactivated organophilic clay gellant of claim 1 wherein the organic cation is a mixture of dimethyl bis(hydrogenated tallow) ammonium and dimethyl benzyl hydrogenated tallow ammonium.

Claim 14

Dependent Claim 36 words

The dry preactivated organophilic clay gellant of claim 1 wherein the preactivating agent is selected from the group consisting of phthalide, o-, m- and p-nitrobenzyl alcohol, o-, m- and p-nitrophenyl alcohol, 1-phenyl-1,2-ethanediol, 1,6-hexanediol and mixtures thereof.

Claim 15

Dependent Claim 15 words

The dry preactivated organophilic clay gellant of claim 13 wherein the preactivating agent is 1,6-hexanediol.

Claim 16

Dependent Claim 20 words

The dry preactivated organophilic clay gellant of claim 1 wherein the moisture content is less than about 5% by weight.

Claim 17

Dependent Claim 20 words

The dry preactivated organophilic clay gellant of claim 15 wherein the moisture content is less than about 2% by weight.

Claim 18

Dependent Claim 176 words

A lubricating grease thickened with a preactivated organophilic clay gellant comprising: (a) a lubricating grease base fluid; (b) a preactivated organophilic clay gellant which is the reaction product of an organophilic clay gellant and a preactivating agent, wherein the amount of preactivated organophilic clay gellant is from about 1 to about 12% by weight of the lubricating grease, said oranophilic clay gellant being the reaction product of a smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay and organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type and said preactivating agent being from about 1 to about 25% by weight of the organophilic clay gellant and being selected form the group consisting of phthalide, 3-hydroxy-4-methoxy benzaldehyde, 4-benzyloxypropiophenone, triethyl citrate, 2-phenoxyethanol, 1-phenyl-1,2-ethanediol, o-, m- and p-nitrobenzyl alcohol, 1,6-hexanediol, castor oil, o-, m- and p-nitrophenethyl alcohol, and mixtures thereof; and (c) water in an amount ranging from about 0.1 to about 10% by weight of the organophilic clay gellant.

Claim 19

Dependent Claim 176 words

A lubricating grease thickened with a preactivated organophilic clay gellant comprising: (a) a lubricating grease base fluid; (b) a preactivated organophilic clay gellant which is the reaction product of an organophilic clay gellant and a preactivating agent, wherein the amount of preactivated organophilic clay gellant is from about 1 to about 12% by weight of the lubricating grease, said oranophilic clay gellant being the reaction product of a smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay and organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type and said preactivating agent being from about 1 to about 25% by weight of the organophilic clay gellant and being selected form the group consisting of phthalide, 3-hydroxy-4-methoxy benzaldehyde, 4-benzyloxypropiophenone, triethyl citrate, 2-phenoxyethanol, 1-phenyl-1,2-ethanediol, o-, m- and p-nitrobenzyl alcohol, 1,6-hexanediol, castor oil, o-, m- and p-nitrophenethyl alcohol, and mixtures thereof; and (c) water in an amount ranging from about 0.1 to about 10% by weight of the organophilic clay gellant.

Claim 20

Dependent Claim 24 words

The lubricating grease of claim 17 wherein the lubricating grease base fluid is a low viscosity index oil or a high viscosity index oil.

Claim 21

Dependent Claim 18 words

The lubricating grease of claim 18 wherein the lubricating grease base fluid is a high viscosity index oil.

Claim 22

Dependent Claim 28 words

The lubricating grease of claim 19 wherein the high viscosity index oil is composed of about 68% paraffinic, about 28% naphthenic and about 4% aromatic components by weight.

Claim 23

Dependent Claim 22 words

The lubricating grease of claim 17 wherein the smectite-type clay is selected from the group consisting of bentonite, hectorite, and mixtures thereof.

Claim 24

Dependent Claim 12 words

The lubricating grease of claim 21 wherein the smectite-type clay is bentonite.

Claim 25

Dependent Claim 28 words

The lubricating grease of claim 17 wherein the amount of organic cation is from about 100 to about 130% of the cation exchange capacity of the smectite-type clay.

Claim 26

Dependent Claim 27 words

The lubricating grease of claim 23 wherein the amount of organic cation is from about 100 to about 116% of the cation exchange capacity of smectite-type clay.

Claim 27

Dependent Claim 28 words

The lubricating grease of claim 17 wherein the organic cation contains at least one lineal or branched, saturated or unsaturated alkyl group having 12 to 22 carbon atoms.

Claim 28

Dependent Claim 135 words

The lubricating grease of claim 25 wherein the organic cation is at least one of ##STR5## wherein X is a nitrogen or phosphorous, Y is sulfur, R 1 is a lineal or branched, saturated or unsaturated alkyl group having 12 to 22 carbon atoms and R 2 , R 3 and R 4 are independently selected from (a) lineal or branched alkyl groups having 1 to 22 carbon atoms; (b) aralkyl group which are benzyl and substituted benzyl moieties including fused ring moieties having lineal or branched 1 to 22 carbon atoms in the alkyl portion of the structure; (c) aryl groups such as phenyl and substituted phenyl including fused ring aromatic substituents; (d) beta, gamma-unsaturated groups having six or less carbon atoms or hydroxylalkyl groups having 2 to 6 carbon atoms; and (e) hydrogen.

Claim 29

Dependent Claim 53 words

The lubricating grease of claim 26 wherein the organic cation is ammonium, R 1 and R 2 are lineal or branched, saturated or unsaturated alkyl groups having 12 to 22 carbon atoms and R 3 and R 4 are lineal or branched, saturated or unsaturated alkyl groups having 1 to 12 carbon atoms.

Claim 30

Dependent Claim 15 words

The lubricating grease of claim 27 wherein the organic cation is dimethyl bis(hydrogenated tallow) ammonium.

Claim 31

Dependent Claim 58 words

The lubricating grease of claim 26 wherein the organic cation is ammonium, R 2 is an aralkyl group having a lineal or branched, saturated or unsaturated alkyl group having 1 to 12 carbons in the alkyl portion and R 3 and R 4 are lineal or branched, saturated or unsaturated alkyl groups having 1 to 12 carbon atoms.

Claim 32

Dependent Claim 16 words

The lubricating grease of claim 29 wherein the organic cation is dimethyl benzyl hydrogenated tallow ammonium.

Claim 33

Dependent Claim 24 words

The lubricating grease of claim 17 wherein the organic cation is a mixture of dimethyl bis(hydrogenated tallow) ammonium and dimethyl benzyl hydrogenated tallow ammonium.

Claim 34

Dependent Claim 33 words

The lubricating grease of claim 17 wherein the preactivating agent is selected from the group consisting of phthalide, o-, m- and p-nitrobenzyl alcohol, o-, m- and p-nitrophenyl alcohol, 1-phenyl-1,2-ethanediol, 1,6-hexanediol and mixtures thereof.

Claim 35

Dependent Claim 12 words

The lubricating grease of claim 32 wherein the preactivating agent is 1,6-hexanediol.

Claim 36

Dependent Claim 27 words

The lubricating grease of claim 17 wherein the amount of preactivated organophilic clay gellant is from about 4 to about 8% by weight of the lubricating grease.

Claim 37

Dependent Claim 26 words

The lubricating grease of claim 17 wherein the amount of water is from about 0.5 to about 6.0% by weight of the preactivated organophilic clay gellant.

Claim 38

Dependent Claim 26 words

The lubricating grease of claim 17 wherein the amount of water is from about 2.0 to about 4.0% by weight of the preactivated organophilic clay gellant.

Claim 39

Dependent Claim 19 words

The lubricating grease of claim 17 wherein the unworked lubricating grease has a cone penetration of 315 or lower.

Claim 40

Dependent Claim 19 words

The lubricating grease of claim 17 wherein the unworked lubricating grease has a cone penetration of 300 or lower.

Claim 41

Dependent Claim 19 words

The lubricating grease of claim 17 wherein the unworked lubricating grease has a cone penetration of 290 or lower.

Claim 42

Dependent Claim 23 words

The lubricating grease of claim 17 wherein the difference in cone penetration values after 60 and 10,000 strokes is less than about 50.

Claim 43

Dependent Claim 23 words

The lubricating grease of claim 17 wherein the difference in cone penetration values after 60 and 10,000 strokes is less than about 25.

Claim 44

Dependent Claim 23 words

The lubricating grease of claim 17 wherein the difference in cone penetration values after 60 and 10,000 strokes is less than about 10.

Claim 45

Dependent Claim 188 words

A process for preparing a preactivated organophilic clay gellant comprising: (a) preparing a slurry of smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay, wherein said clay is dispersed in water at a concentration of from about 0.5 to abut 80% by weight; (b) subjecting the slurry to high shear conditions whereby clay agglomerates are separated; (c) reacting the smectite-type clay with organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type clay whereby at least some of the cation exchange sites of the smectite-type clay are substituted with organic cation thereby forming an organophilic clay gellant; and (d) reacting the organophilic clay gellant with a preactivating agent in an amount of from about 1 to about 25% by weight of the organophilic clay gellant and having at least one active group selected from the group consisting of carboxyl, hydroxyl, primary amine, secondary amine, tertiary amine, aldehyde, ketone, ether, ester, nitro and sulfo whereby the resultant preactivated organophilic clay gellant exhibits an increase in d-spacing of at least one angstrom.

Claim 46

Dependent Claim 188 words

A process for preparing a preactivated organophilic clay gellant comprising: (a) preparing a slurry of smectite-type clay having a cation exchange capacity of at least 75 milliequivalents per 100 grams of clay, wherein said clay is dispersed in water at a concentration of from about 0.5 to abut 80% by weight; (b) subjecting the slurry to high shear conditions whereby clay agglomerates are separated; (c) reacting the smectite-type clay with organic cation in an amount ranging from about 90 to about 150% of the cation exchange capacity of the smectite-type clay whereby at least some of the cation exchange sites of the smectite-type clay are substituted with organic cation thereby forming an organophilic clay gellant; and (d) reacting the organophilic clay gellant with a preactivating agent in an amount of from about 1 to about 25% by weight of the organophilic clay gellant and having at least one active group selected from the group consisting of carboxyl, hydroxyl, primary amine, secondary amine, tertiary amine, aldehyde, ketone, ether, ester, nitro and sulfo whereby the resultant preactivated organophilic clay gellant exhibits an increase in d-spacing of at least one angstrom.

Claim 47

Dependent Claim 36 words

The process of claim 43 wherein the sheared clay exhibits an increase in cation exchange capacity of from about 10 to about 50% as determined by the methylene blue spot test when compared to unsheared clay.

Claim 48

Dependent Claim 36 words

The process of claim 44 wherein the sheared clay exhibits an increase in cation exchange capacity of from about 15 to about 40% as determined by the methylene blue spot test when compared to unsheared clay.

Claim 49

Dependent Claim 28 words

The process of claim 43 wherein the sheared clay exhibits a reduction in median particle size of from about 10 to about 80% when compared to unsheared clay.

Claim 50

Dependent Claim 28 words

The process of claim 46 wherein the sheared clay exhibits a reduction in median particle size of from about 20 to about 60% when compared to unsheared clay.

Claim 51

Dependent Claim 33 words

The process of claim 43 wherein the high shear conditions are achieved by passing the slurry at least one time through a Manton-Gaulin homogenizer operating at from about 500 to about 8,000 psi.

Claim 52

Dependent Claim 31 words

The process of claim 43 wherein the smectite-type clay and the organic cation are reacted in a slurry containing from about 0.5 to about 2.5% by weight of the smectite-type clay.

Claim 53

Dependent Claim 21 words

The process of claim 49 wherein the slurry contains from about 0.5 to about 2% by weight of the smectite-type clay.

Claim 54

Dependent Claim 19 words

The process of claim 43 wherein the organophilic clay gellant is dried prior to reaction with the preactivating agent.

Claim 55

Dependent Claim 26 words

The process of claim 51 wherein the organophilic clay gellant is dried such that the temperature of the organophilic clay gellant does not exceed 80° C.

Claim 56

Dependent Claim 22 words

The process of claim 52 wherein the organophilic clay gellant is dried in an airstream of from 0° to about 80° C.

Claim 57

Dependent Claim 22 words

The process of claim 53 wherein the organophilic clay gellant is dried in an airstream of from 0° to about 50° C.

Claim 58

Dependent Claim 16 words

The process of claim 52 wherein the organophilic clay gellant is dried in a fluidized bed.

Claim 59

Dependent Claim 13 words

The process of claim 52 wherein the organophilic clay gellant is freeze dried.

Claim 60

Dependent Claim 20 words

The process of claim 51 wherein the preactivating agent is reacted with the dry organophilic clay gellant by dry mixing.

Claim 61

Dependent Claim 34 words

The process of claim 51 wherein the preactivating agent is reacted with the dry organophilic clay gellant by contacting with melted preactivating agent or by contact with a liquid dispersion of the preactivating agent.

Claim 62

Dependent Claim 18 words

The process of claim 43 wherein the organophilic clay gellant is wet when reacted with the preactivating agent.

Claim 63

Dependent Claim 24 words

The process of claim 59 wherein the preactivating agent is formed into a liquid dispersion which is contacted with the wet organophilic clay gellant.

Claim 64

Dependent Claim 28 words

The process of claim 59 wherein the preactivated organophilic clay gellant is dried such that the temperature of the preactivated organophilic clay gellant does not exceed 80° C.

Claim 65

Dependent Claim 23 words

The process of claim 61 wherein the preactivated organophilic clay gellant is dried in an airstream of from 0° to about 80° C.

Claim 66

Dependent Claim 23 words

The process of claim 62 wherein the preactivated organophilic clay gellant is dried in an airstream of from 0° to about 50° C.

Claim 67

Dependent Claim 17 words

The process of claim 61 wherein the preactivated organophilic clay gellant is dried in a fluidized bed.

Claim 68

Dependent Claim 14 words

The process of claim 61 wherein the preactivated organophilic clay gellant is freeze dried.

Claim 69

Dependent Claim 27 words

The process of claim 43 wherein the organophilic clay gellant is dried at a temperature above about 80° C. and then dry milled with the preactivating agent.

Claim 70

Dependent Claim 40 words

The process of claim 43 wherein the preactivating agent is selected from the group consisting of phthalide, 3-hydroxy-4-methoxy benzaldehyde, 4-benzyloxypropiophenone, triethyl citrate, 2-phenoxyethanol, 1-phenyl-1,2-ethanediol, o-, m- and p-nitrobenzyl alcohol, 1,6-hexanediol, castor oil, o-, m- and p-nitrophenethyl alcohol, and mixtures thereof.

Claim 71

Dependent Claim 28 words

The process of claim 67 wherein the preactivating agent is selected from phthalide, o-, m- and p-nitrobenzyl alcohol, o-, m- and p-nitrophenyl alcohol, 1-phenyl-1,2-ethanediol, 1,6-hexanediol and mixtures thereof.

Claim 72

Dependent Claim 11 words

The process of claim 68 wherein the preactivating agent is 1,6-hexanediol.

Claim 73

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 43.

Claim 74

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 49.

Claim 75

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 51.

Claim 76

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 52.

Claim 77

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 57.

Claim 78

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 59.

Claim 79

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 67.

Claim 80

Dependent Claim 12 words

The preactivated organophilic clay gellant prepared by the process of claim 69.

Claim 81

Dependent Claim 35 words

The dry preactivated organophilic clay gellant of claim 1 wherein the amount of preactivating agent reacted with the organophilic clay gellant is from about 3 to about 17% by weight of the organophilic clay gellant.

Claim 82

Dependent Claim 28 words

The dry preactivated organophilic clay gellant of claim 14 wherein the amount of 1,6-hexanediol is from about 1 to about 18% by weight of the organophilic clay gellant.

Claim 83

Dependent Claim 28 words

The dry preactivated organophilic clay gellant of claim 79 wherein the amount of 1,6-hexanediol is from about 3 to about 14% by weight of the organophilic clay gellant.

Claim 84

Dependent Claim 28 words

The dry preactivated organophilic clay gellant of claim 80 wherein the amount of 1,6-hexanediol is from about 4 to about 12% by weight of the organophilic clay gellant.

Claim 85

Dependent Claim 33 words

The lubricating grease of claim 17 wherein the amount of preactivating agent reacted with the organophilic clay gellant (b) is from about 3 to about 17% by weight of the organophilic clay gellant.

Claim 86

Dependent Claim 32 words

The process of claim 43 wherein the amount of preactivating agent reacted with the organophilic clay gellant (d) is from about 3 to about 17% by weight of the organophilic clay gellant.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1990-05-11	1990-11-10	1991-05-12	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1994-05-11	1994-11-10	1995-05-12	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1998-05-11	1998-11-10	1999-05-12	$7700.00	Window Closed / Lapsed

Preactivated organophilic clay gellant lubricating grease thickened with preactivated organophilic clay gellant and process for preparing preactivated organophilic clay gellants

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