US4818508A — Process for preparing molecular sieve bodies

Claim 1

Independent Claim 72 words

A method of preparing molecular sieves of the zerolite type in massive bodies which comprises digesting in the presence of alkali metal oxide massive preformed or shaped bodies, which contain reactive clay and which are prepared from particles of non-reactive clay, in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns, until said reactive clay is substantially converted to crystalline zeolite.

Claim 2

Independent Claim 72 words

A method of preparing molecular sieves of the zerolite type in massive bodies which comprises digesting in the presence of alkali metal oxide massive preformed or shaped bodies, which contain reactive clay and which are prepared from particles of non-reactive clay, in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns, until said reactive clay is substantially converted to crystalline zeolite.

Claim 3

Dependent Claim 14 words

A method according to claim 1 wherein said reactive clay is metakaolin or metahalloysite.

Claim 4

Dependent Claim 29 words

A method according to claim 1 wherein at least fifty weight percent (50%) of the particles in said clay range in size from about 2 to about 10 microns.

Claim 5

Independent Claim 148 words

A method of preparing molecular sieves of the zeolite type in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting in the presence of aqueous alkali metal oxide said thermally treated shaped bodies until said reaction form of clay is substantially converted to pure crystalline zeolite.

Claim 6

Independent Claim 148 words

A method of preparing molecular sieves of the zeolite type in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting in the presence of aqueous alkali metal oxide said thermally treated shaped bodies until said reaction form of clay is substantially converted to pure crystalline zeolite.

Claim 7

Dependent Claim 13 words

A method according to claim 4 wherein said clay is kaolinite or halloysite.

Claim 8

Dependent Claim 29 words

A method according to claim 4 wherein at least fifty weight percent (50%) of the particles in said clay range in size from about 2 to about 10 microns.

Claim 9

Dependent Claim 33 words

A method according to claim 4 wherein said pore generating material is present at a level of from about one percent (1%) to about twenty-five percent (25%) by weight relative to said clay.

Claim 10

Dependent Claim 29 words

A method according to claim 7 wherein said pore generating material is present at a level of from about two percent (2%) to about thirteen percent (13%) by weight.

Claim 11

Dependent Claim 37 words

A method according to claim 4 wherein said pore generating material is selected from the group consisting of sawdust, powdered carbon, coke, lampblack, cellulose products, starches, hydrocarbon polymer fibers, and polymeric materials containing hydrogen, carbon and oxygen.

Claim 12

Dependent Claim 17 words

A method according to claim 9 wherein said pore generating material is smaller than about 149 microns.

Claim 13

Dependent Claim 23 words

A method according to claim 4 wherein said mixture contains from about thirty-five percent (35%) to about forty-five percent (45%) by weight water.

Claim 14

Dependent Claim 23 words

A method according to claim 11 wherein said mixture contains from about thirty-eight percent (38%) to about forty-two percent (42%) by weight water.

Claim 15

Dependent Claim 68 words

A method according to claim 4 wherein said mixture comprises: (a) from about fifty-five percent (55%) to about sixty-five percent (65%) by weight of a dry mixture containing from about seventy percent (70%) to about ninety percent (90%) clay and from about two percent (2%) to about twenty percent (20%) pore generating material; and (b) from about thirty-five percent (35%) to about forty-five percent (45%) by weight water.

Claim 16

Dependent Claim 24 words

A method according to claim 13 wherein said thermally treated shaped bodies exhibit a piece density of from about 1.0 to about 1.3 g/cc.

Claim 17

Dependent Claim 20 words

A method according to claim 14 wherein said piece density ranges in value from about 1.05 to about 1.25 g/cc.

Claim 18

Dependent Claim 65 words

A method according to claim 4 wherein said mixture comprises a wet strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite and kaolinite, whose particles are smaller than about one micron in size and which exhibit binding properties for clay particles, which is present as from about one percent (1%) to about ten percent (10%) by weight.

Claim 19

Dependent Claim 27 words

A method according to claim 16 wherein said wet strength enhancing agent is present as from about two percent (2%) to about seven percent (7%) by weight.

Claim 20

Dependent Claim 43 words

A method according to claim 4 wherein said mixture is formed into shaped bodies by extruding, spray drying, prilling, molding, casting, slip casting, tableting, briquetting, or bead forming methods selected from the group consisting of tumbling, drum rolling, Nauta mixing and disk forming.

Claim 21

Dependent Claim 22 words

A method according to claim 18 wherein said mixture is formed into shaped bodies by extruding, spray drying, prilling or bead forming.

Claim 22

Dependent Claim 28 words

A method according to claim 4 wherein said mixture further comprises from about one percent (1%) to about forthy percent (40%) by weight reactive clay or zeolite particles.

Claim 23

Independent Claim 176 words

A method of preparing molecular sieves of zeolite A in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including both solid and liquid phases, may be approximately expressed in terms of mole ratio of oxides as: M.sub.2 O/SiO.sub.2 =0.5-1.5 SiO.sub.2 /Al.sub.2 O.sub.3 1.6-2.2 H.sub.2 O/M.sub.2 O=10-100 until said reactive form of clay is substantially converted to crystalline zeolite A.

Claim 24

Independent Claim 176 words

A method of preparing molecular sieves of zeolite A in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including both solid and liquid phases, may be approximately expressed in terms of mole ratio of oxides as: M.sub.2 O/SiO.sub.2 =0.5-1.5 SiO.sub.2 /Al.sub.2 O.sub.3 1.6-2.2 H.sub.2 O/M.sub.2 O=10-100 until said reactive form of clay is substantially converted to crystalline zeolite A.

Claim 25

Dependent Claim 76 words

A method according to claim 21 wherein said mixture to be shaped further comprises a wet strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite and kaolinite, whose particles are smaller than about one micron in size and which exhibit binding properties for clay particles, which is present in an amount in value from about one percent (1%) to about ten percent (10%) by weight of dry ingredients.

Claim 26

Dependent Claim 30 words

A method according to claim 22 wherein said wet strength enhancing agent is present in an amount of from about two percent (2%) to about seven percent (7%) by weight.

Claim 27

Dependent Claim 37 words

A method according to claim 21 wherein said pore generating material is selected from the group consisting of sawdust, powdered carbon, coke, lampblack, cellulose products, starches, hydrocarbon polymer fibers and polymeric materials containing hydrogen, carbon and oxygen.

Claim 28

Dependent Claim 82 words

A method according to claim 21 wherein said mixture comprises: (a) from about fifty-five percent (55%) to about sixty-five percent (65%) by weight of a dry mixture containing from about seventy percent (70%) to about ninety percent (90%) clay, from about two percent (2%) to about fifteen percent (15%) pore generating material, and from about two percent (2%) to about seven percent (7%) wet strength enhancing agent; and (b) from about thirty-five percent (35%) to about forty-five percent (45%) by weight water.

Claim 29

Independent Claim 176 words

A method of preparing molecular sieves of zeolite X in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including liquid and solid phases, may be approximately expressed, in terms of mole ratio of oxides as: M.sub.2 O/SiO.sub.2 =0.8-1.5 SiO.sub.2 /Al.sub.2 O.sub.3 =2.5 -5 H.sub.2 O/M.sub.2 O=25-60 until said reactive form of clay is substantially converted to crystalline zeolite X.

Claim 30

Independent Claim 176 words

A method of preparing molecular sieves of zeolite X in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including liquid and solid phases, may be approximately expressed, in terms of mole ratio of oxides as: M.sub.2 O/SiO.sub.2 =0.8-1.5 SiO.sub.2 /Al.sub.2 O.sub.3 =2.5 -5 H.sub.2 O/M.sub.2 O=25-60 until said reactive form of clay is substantially converted to crystalline zeolite X.

Claim 31

Dependent Claim 31 words

A method according to claim 26 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to the mixture to be shaped.

Claim 32

Dependent Claim 31 words

A method according to claim 27 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel and reactive particulate silica.

Claim 33

Dependent Claim 36 words

A method according to claim 26 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to the liquid phase of said reaction medium of step c.

Claim 34

Dependent Claim 31 words

A method according to claim 29 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel or reactive particulate silica.

Claim 35

Dependent Claim 37 words

A method according to claim 26 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to both said mixture to be shaped and to said reaction medium.

Claim 36

Dependent Claim 31 words

A method according to claim 31 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel and reactive particulate silica.

Claim 37

Dependent Claim 77 words

A method according to claim 26 wherein said mixture to be shaped further comprises a wet strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite and kaolinite, whose particles are smaller than about one micron in said and which exhibit binding properties for clay particles, which is present in an amount ranging in value from about one percent (1%) to about ten percent (10%) by weight of dry ingredients.

Claim 38

Dependent Claim 31 words

A method according to claim 26 wherein said mixture to be shaped further comprises from about one percent (1%) to about forty percent (40%) by weight reactive clay or zeolite particles.

Claim 39

Dependent Claim 32 words

A method according to claim 26 wherein said mixture to be shaped further comprises from about five percent (5%) to about twenty percent (20%) by weight colloidal, solid or reactive particulate silica.

Claim 40

Dependent Claim 40 words

A method according to claim 26 wherein said reaction medium for digestion contains alkali metal silicate in an amount ranging in value from about two percent (22%) to about ten percent (10%) by weight of total aluminosilicate and pore generator.

Claim 41

Dependent Claim 37 words

A method according to claim 26 wherein said pore generating material is selected from the group consisting of sawdust, powdered carbon, coke, lampblack, cellulose products, starches, hydrocarbon polymer fibers and polymeric materials containing hydrogen, carbon and oxygen.

Claim 42

Dependent Claim 101 words

A method according to claim 26 wherein said mixture to be shaped comprises: (a) from about fifty-five percent (55%) to about sixty-five percent (65%) by weight of a dry mixture containing from about seventy percent (70%) to about ninety percent (90%) clay, from about three percent (3%) to about twenty percent (20%) pore generating material, from about two percent (2%) to about seven percent (7%) wet strength enhancing agent, and from about five percent (5%) to about twenty percent (20%) colloidal, solid or reactive particulate silica; and (b) from about thirty-five percent (35%) to about forty-five percent (45%) by weight water.

Claim 43

Independent Claim 175 words

A method of preparing molecular sieves of zeolite Y in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including liquid and solid phases, may be approximately expressed, in terms of mole ratio of oxides, as: M.sub.2 O/SiO.sub.2 =0.3-0.6 SiO.sub.2 /Al.sub.2 O.sub.3 =6-9 H.sub.2 O/M.sub.2 O=35-50 until said reactive form of clay is substantially converted to crystalline zeolite Y.

Claim 44

Independent Claim 175 words

A method of preparing molecular sieves of zeolite Y in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to a reactive form; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting said thermally treated shaped bodies in an aqueous alkaline reaction medium whose overall composition, including liquid and solid phases, may be approximately expressed, in terms of mole ratio of oxides, as: M.sub.2 O/SiO.sub.2 =0.3-0.6 SiO.sub.2 /Al.sub.2 O.sub.3 =6-9 H.sub.2 O/M.sub.2 O=35-50 until said reactive form of clay is substantially converted to crystalline zeolite Y.

Claim 45

Dependent Claim 31 words

A method according to claim 39 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to the mixture to be shaped.

Claim 46

Dependent Claim 31 words

A method according to claim 40 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel and reactive particulate silica.

Claim 47

Dependent Claim 36 words

A method according to claim 39 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to the liquid phase of said reaction medium of step c.

Claim 48

Dependent Claim 31 words

A method according to claim 42 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel and reactive particulate silica.

Claim 49

Dependent Claim 37 words

A method according to claim 39 wherein said mole ratio of SiO 2 /Al 2 O 3 is achieved by addition of a silica source to both said mixture to be shaped and to said reaction medium.

Claim 50

Dependent Claim 31 words

A method according to claim 44 wherein said silica source is selected from the group consisting of colloidal silica sol, silicic acid, alkali metal silicate, silica gel and reactive particulate silica.

Claim 51

Dependent Claim 77 words

A method according to claim 39 wherein said mixture to be shaped further comprises a wet strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite and kaolinite, whose particles are smaller than about one micron in size and which exhibit binding propoerties for clay particles, which is present in an amount ranging in value from about one percent (1%) to about ten percent (10%) by weight of dry ingredients.

Claim 52

Dependent Claim 31 words

A method according to claim 39 wherein said mixture to be shaped further comprises from about one percent (1%) to about forty percent (40%) by weight reactive clay or zeolite particles.

Claim 53

Dependent Claim 29 words

A method according to claim 39 wherein said mixture to be shaped further comprises from about eight percent (8%) to about thirty percent (30%) by weight solid silica source.

Claim 54

Dependent Claim 41 words

A method according to claim 39 wherein said reaction medium for digestion contains alkali metal silicate in an amount ranging in value from about three percent (3%) to about fifteen percent (15%) by weight of total aluminosilicate and pore generator weight.

Claim 55

Dependent Claim 37 words

A method according to claim 39 wherein said pore generating material is selected from the group consisting of sawdust, powdered carbon, coke, lampblack, cellulose products, starches, hydrocarbon polymer fibers and polymeric materials containing hydrogen, carbon and oxygen.

Claim 56

Dependent Claim 101 words

A method according to claim 39 wherein said mixture to be shaped comprises: (a) from about fifty-five percent (55%) to about sixty-five percent (65%) by weight of a dry mixture containing from about seventy percent (70%) to about ninety percent (90%) clay, from about three percent (3%) to about twenty percent (20%) pore generating material, from about two percent (2%) to about seven percent (7%) wet strength enhancing agent, and from about eight percent (8%) to about thirty percent (30%) colloidal, solid or reactive particulate silica; and (b) from about thirty-five percent (35%) to about forty-five percent (45%) by weight water.

Claim 57

Independent Claim 126 words

A method of preparing molecular sieves of the zeolite type in massive bodies, which method comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies during digestion, wherein said material is water soluble after the thermal treatment in step b below; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to convert said clay to a reactive form; and c. digesting said thermally treated shaped bodies in an aqueous alkaline medium under conditions of time, temperature and concentration sufficient to convert substantially all of said reactive form of clay into crystalline zeolite.

Claim 58

Independent Claim 126 words

A method of preparing molecular sieves of the zeolite type in massive bodies, which method comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies during digestion, wherein said material is water soluble after the thermal treatment in step b below; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to convert said clay to a reactive form; and c. digesting said thermally treated shaped bodies in an aqueous alkaline medium under conditions of time, temperature and concentration sufficient to convert substantially all of said reactive form of clay into crystalline zeolite.

Claim 59

Dependent Claim 42 words

A method according to claim 52 wherein said pore generating material is selected from the group consisting of the water-soluble carbonates, bicarbonates, phosphates, chlorides, nitrates, sulfates and acetate salts of alkali metals, alkaline earths, transition metals, rare earth metals, ammonium and aluminum.

Claim 60

Dependent Claim 38 words

A method according to claim 52 wherein said pore generating material is present in an amount ranging in value from about three percent (3%) to about twenty percent (20%) by weight of the dry ingredients in said mixture.

Claim 61

Independent Claim 162 words

A method of preparing molecular sieves of the zeolites A, X, and Y in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 microns to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies during digestion; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to convert said clay to a reactive form; and c. digesting said thermally treated shaped bodies in an aqueous alkaline medium whose overall composition, including both solid and liquid phases, may be approximately expressed in terms of moles of oxide by the values given in Table 1 at a temperature and for a time sufficient to convert substantially all of said reactive form of clay to crystalline zeolite.

Claim 62

Independent Claim 162 words

A method of preparing molecular sieves of the zeolites A, X, and Y in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay in which at least fifty weight percent (50%) of the particles range in size from about 1.5 microns to about 15 microns; ii. pore generating material in sufficient quantity to provide substantial porosity in said shaped bodies during digestion; and iii. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to convert said clay to a reactive form; and c. digesting said thermally treated shaped bodies in an aqueous alkaline medium whose overall composition, including both solid and liquid phases, may be approximately expressed in terms of moles of oxide by the values given in Table 1 at a temperature and for a time sufficient to convert substantially all of said reactive form of clay to crystalline zeolite.

Claim 63

Dependent Claim 22 words

A method according to claim 55 wherein said pore generating material is a material that is water soluble after said thermal treatment.

Claim 64

Dependent Claim 41 words

A method according to claim 56 wherein said pore generating material is selected from the group consisting of the carbonate, bicarbonate, phosphate, chloride, nitrate, sulfate and acetate salts of alkali metals, alkaline earths, transition metals, rare earth metals, ammonium and aluminum.

Claim 65

Dependent Claim 38 words

A method according to claim 55 wherein said pore generating material is present in an amount ranging in value from about three percent (3%) to about twenty percent (20%) by weight of the dry ingredients in said mixture.

Claim 66

Dependent Claim 48 words

A method according to claim 52 wherein said mixture further comprises a wet-strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite andkaolinite, whose particles are smaller than about one micron in size and which exhibit binding properties for clay particles.

Claim 67

Dependent Claim 73 words

A method according to claim 55 wherein said mixture further comprises a wet-strength enhancing agent selected from clays selected from the group consisting of attapulgite, montmorillonite, halloysite, sepiolite, palygorskite and kaolinite, whose particles are smaller than about one micron in size and which exhibit binding properties for clay particles, which is present in an amount ranging in value from about one percent (1%) to about ten percent (10%) by weight of dry ingredients.

Claim 68

Dependent Claim 16 words

A method according to claim 1 wherein said clay has the general formula Al.sub.2 O.sub.3.2SiO.sub.2.2-4H.sub.2 O.

Claim 69

Dependent Claim 24 words

A method according to claim 28 wherein a colloidal silica sol and a reactive particulate silica are added to said mixture to be shaped.

Claim 70

Dependent Claim 35 words

A method according to claim 32 wherein a colloidal silica sol and a reactive particulate silica are added to said mixture to be shaped and an alkali metal silicate is added to said reaction medium.

Claim 71

Dependent Claim 24 words

A method according to claim 41 wherein a colloidal silica sol and a reactive particulate silica are added to said mixture to be shaped.

Claim 72

Dependent Claim 35 words

A method according to claim 46 wherein a colloidal silica sol and a reactive particulate silica are added to said mixture to be shaped and an alkali metal silicate is added to said reaction medium.

Claim 73

Independent Claim 193 words

A method of preparing molecular sieves of the zeolite type in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay having the general formula Al 2 O 3 .SiO 2 .2-4H 2 O in which at least fifty weight percent (50%) of the particles range in size from about 2 to about 10 microns; ii. a wet strength enhancing agent comprising an attapulgite clay whose particles are small than about one micron in size; iii. pore generating materials in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iv. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to an amorphous reactive form which can be converted to crystalline aluminosilicates of the zeolite type; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting in the presence of aqueous alkali metal oxide said thermally treated shaped bodies until said reactive form of clay is substantially converted to pure crystalline zeolite.

Claim 74

Independent Claim 193 words

A method of preparing molecular sieves of the zeolite type in massive bodies which comprises: a. forming into massive preformed or shaped bodies a mixture comprising: i. non-reactive clay having the general formula Al 2 O 3 .SiO 2 .2-4H 2 O in which at least fifty weight percent (50%) of the particles range in size from about 2 to about 10 microns; ii. a wet strength enhancing agent comprising an attapulgite clay whose particles are small than about one micron in size; iii. pore generating materials in sufficient quantity to provide substantial porosity in said shaped bodies after thermal treatment; and iv. water in sufficient quantity to provide plasticity; b. thermally treating said shaped bodies at a temperature and for a time sufficient to: i. convert said non-reactive clay to an amorphous reactive form which can be converted to crystalline aluminosilicates of the zeolite type; and ii. generate substantial porosity in said shaped bodies by destroying substantially all of said pore generating material; and c. digesting in the presence of aqueous alkali metal oxide said thermally treated shaped bodies until said reactive form of clay is substantially converted to pure crystalline zeolite.

Claim 75

Dependent Claim 38 words

A method according to claim 67 wherein said mixture of a. further comprises pore generating material which is water soluble after said thermal treatment and thus provides additional porosity in said shaped bodies during the digestion of c.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1992-04-03	1992-10-03	1993-04-04	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1996-04-03	1996-10-03	1997-04-04	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2000-04-03	2000-10-03	2001-04-04	$7700.00	Window Closed / Lapsed

Process for preparing molecular sieve bodies

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