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US4542002A Expired / Lapsed US ⏱️ 0.0 years remaining

Silicates with high ion exchange capacity derived from sepiolite and processes for their production

Assignee: SYNTHESIS ENGINEERING Ltd SUITE 1601 7 KING ST EAST TORONTO ONTARIO CANADA M5C 1A2
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Filing: 1983-02-28
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Granted: 1985-09-17
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Expires: 2003-02-28
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Abstract

Abstract Silicate having high ion exchange capacity are obtained by reacting sepiolites with a base, preferably a strong base in the presence of a polar liquid at a temperature, preferably elevated, and for a period sufficient to increase the ion exchange capacity to at least 50 meq. per 100 g, more preferably at least 100 meq. per 100 g. In the preferred form, the reaction is carried out at above 100° C. in an autoclave.

Inventors

  • 👤 Avelino C. Corma
  • 👤 Amparo C. Mifsud
  • 👤 Joaquin P. Perez

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 00:27
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/36

Claims Analysis

Total Claims: 24
Claim 1
Independent Claim 102 words
A process for obtaining a silicate derived from a sepiolite comprising reacting said sepiolite with a base selected from the group consisting of alkali metal hydroxides, alkaline earth metal hydroxides and ammonium hydroxide, in the presence of a polar liquid selected from the group consisting of water, alcohols and mixtures thereof, at a temperature in the range from about 100° C. to about 400° C. and for a period sufficient to increase the ion exchange capacity of the sepiolite to at least 100 meq. per 100 g with respect to potassium or magnesium, and recovering a silicate with said ion exchange capacity.
Claim 2
Dependent Claim 102 words
A process for obtaining a silicate derived from a sepiolite comprising reacting said sepiolite with a base selected from the group consisting of alkali metal hydroxides, alkaline earth metal hydroxides and ammonium hydroxide, in the presence of a polar liquid selected from the group consisting of water, alcohols and mixtures thereof, at a temperature in the range from about 100° C. to about 400° C. and for a period sufficient to increase the ion exchange capacity of the sepiolite to at least 100 meq. per 100 g with respect to potassium or magnesium, and recovering a silicate with said ion exchange capacity.
Claim 3
Dependent Claim 15 words
A process as claimed in claim 1 wherein the base is an alkali metal hydroxide.
Claim 4
Dependent Claim 39 words
A process as claimed in claim 1 wherein the weight ratio of sepiolite to polar liquid is between about 0.01:1 and about 1:1, and the weight ratio of sepiolite to said hydroxide is between about 0.25:1 and about 40:1.
Claim 5
Dependent Claim 39 words
A process as claimed in claim 3 wherein the weight ratio of sepiolite to polar liquid is between about 0.05:1 and about 0.5:1 and the weight ratio of sepiolite to said hydroxide is between about 1.5:1 and about 15:1.
Claim 6
Dependent Claim 18 words
A process as claimed in claim 1 wherein said temperature is about 100° C. to about 200° C.
Claim 7
Dependent Claim 20 words
A process as claimed in claim 1 carried out above the boiling point of the polar liquid in an autoclave.
Claim 8
Dependent Claim 20 words
A process as claimed in claim 1 wherein the reaction time is between about 5 minutes and about 20 days.
Claim 9
Dependent Claim 18 words
A process as claimed in claim 7 wherein said time is about 2 hours to about 8 days.
Claim 10
Dependent Claim 14 words
A process as claimed in claim 1 carried out in the presence of agitation.
Claim 11
Dependent Claim 43 words
A process as claimed in claim 1 carried out in the presence of a member selected from the group consisting of alkali metal carbonates, alkaline earth metal carbonates, alkaline earth metal carbonates, and ammonium carbonate, said member being added to the reaction mixture.
Claim 12
Dependent Claim 14 words
A process as claimed in claim 1 carried out in an agitated batch reactor.
Claim 13
Dependent Claim 34 words
A process as claimed in claim 1 wherein the starting material sepiolite is a natural sepiolite pretreated with a pretreatment agent selected from the group consisting of mineral acids, organic acids and ammonium salts.
Claim 14
Dependent Claim 18 words
A process as claimed in claim 1 including the steps of filtering, washing and calcining the product silicate.
Claim 15
Dependent Claim 129 words
A silicate having an ion exchange capacity with respect to magnesium of at least about 100 meq. per 100 g and conforming to the general formula Si.sub.y W.sub.w M.sub.x A.sub.z O.sub.30 (OH).sub.4 wherein W is selected from the group consisting of aluminum, magnesium, iron, nickel, manganese and mixtures thereof; M is a divalent metal selected from the group consisting of the alkaline earth metals, and mixtures thereof; A is selected from the group consisting of alkali metals, ammonium ion and mixtures thereof; y is from about 10 to about 12; w is from about 3.5 to about 8; x is from about 0 to about 2; z is from greater than zero up to about 4; and the molar ratio w:y is from about 0.29:1 up to about 0.8:1.
Claim 16
Dependent Claim 129 words
A silicate having an ion exchange capacity with respect to magnesium of at least about 100 meq. per 100 g and conforming to the general formula Si.sub.y W.sub.w M.sub.x A.sub.z O.sub.30 (OH).sub.4 wherein W is selected from the group consisting of aluminum, magnesium, iron, nickel, manganese and mixtures thereof; M is a divalent metal selected from the group consisting of the alkaline earth metals, and mixtures thereof; A is selected from the group consisting of alkali metals, ammonium ion and mixtures thereof; y is from about 10 to about 12; w is from about 3.5 to about 8; x is from about 0 to about 2; z is from greater than zero up to about 4; and the molar ratio w:y is from about 0.29:1 up to about 0.8:1.
Claim 17
Dependent Claim 13 words
A silicate as claimed in claim 14 wherein A is an alkali metal.
Claim 18
Dependent Claim 11 words
A silicate as claimed in claim 15 wherein A is sodium.
Claim 19
Dependent Claim 16 words
A silicate as claimed in claim 14 wherein z is from about 1 to about 2.
Claim 20
Dependent Claim 148 words
A silicate in sodium form having been calcined at 250° C. and having the formula Si y W x M x Na z O 30 (OH) 4 , wherein W is selected from the group consisting of aluminum, magnesium, iron, nickel, manganese and mixtures thereof; M is a divalent metal selected from the group consisting of alkaline earth metals, and mixtures thereof; y is from about 10 to about 12, w is from about 3.5 to about 8; x is from about 0 to about 2; and z is from greater than zero up to about 4; and having the following X-ray difractogram: ______________________________________ 20 d(A) I.sub.obs hkl ______________________________________ 6.9 12.80 s 110 19.7 4.50 w 060 20.4 4.34 i 131 26.5 3.35 i 080 34.4 2.60 w 441,281 35.2 2.54 w 371,191 36.5 2.45 w 202,042 ______________________________________ wherein the relative intensities are ms=strongest, s=strong, i=intermediate and w=weak.
Claim 21
Dependent Claim 148 words
A silicate in sodium form having been calcined at 250° C. and having the formula Si y W x M x Na z O 30 (OH) 4 , wherein W is selected from the group consisting of aluminum, magnesium, iron, nickel, manganese and mixtures thereof; M is a divalent metal selected from the group consisting of alkaline earth metals, and mixtures thereof; y is from about 10 to about 12, w is from about 3.5 to about 8; x is from about 0 to about 2; and z is from greater than zero up to about 4; and having the following X-ray difractogram: ______________________________________ 20 d(A) I.sub.obs hkl ______________________________________ 6.9 12.80 s 110 19.7 4.50 w 060 20.4 4.34 i 131 26.5 3.35 i 080 34.4 2.60 w 441,281 35.2 2.54 w 371,191 36.5 2.45 w 202,042 ______________________________________ wherein the relative intensities are ms=strongest, s=strong, i=intermediate and w=weak.
Claim 22
Dependent Claim 155 words
A silicate in nickel form having been calcined at 250° C. and having the formula Si y Ni w M x A z O 30 (OH) 4 , wherein M is a divalent metal selected from the group consisting of alkaline earth metals, and mixtures thereof; A is selected from the group consisting of alkali metals, ammonium ion and mixtures thereof; y is from about 10 to about 12, w is from about 3.5 to about 8, x is from about 0 to about 2, and z is from greater than zero up to about 4, and having the following X-ray difractogram: ______________________________________ 20 d(A) I.sub.obs hkl ______________________________________ 7.10 12.44 s 110 17.54 5.05 w 150 19.64 4.51 i 060 20.50 4.32 i 131 23.60 3.76 w 260 26.46 3.36 i 080 27.70 3.21 w 331 34.60 2.59 i 371,191 36.50 2.45 w 202,042 ______________________________________ wherein the relative intensities are ms=strongest, s=strong, i=intermediate and w=weak.
Claim 23
Dependent Claim 155 words
A silicate in nickel form having been calcined at 250° C. and having the formula Si y Ni w M x A z O 30 (OH) 4 , wherein M is a divalent metal selected from the group consisting of alkaline earth metals, and mixtures thereof; A is selected from the group consisting of alkali metals, ammonium ion and mixtures thereof; y is from about 10 to about 12, w is from about 3.5 to about 8, x is from about 0 to about 2, and z is from greater than zero up to about 4, and having the following X-ray difractogram: ______________________________________ 20 d(A) I.sub.obs hkl ______________________________________ 7.10 12.44 s 110 17.54 5.05 w 150 19.64 4.51 i 060 20.50 4.32 i 131 23.60 3.76 w 260 26.46 3.36 i 080 27.70 3.21 w 331 34.60 2.59 i 371,191 36.50 2.45 w 202,042 ______________________________________ wherein the relative intensities are ms=strongest, s=strong, i=intermediate and w=weak.
Claim 24
Dependent Claim 13 words
A process as claimed in claim 12 wherein said pretreatment agent is EDTA.

References Cited (Backward Citations)

US3428568A Cited
US4169774A Cited
US4469807A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1988-09-16 1989-03-18 1989-09-17 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1992-09-16 1993-03-18 1993-09-17 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1996-09-16 1997-03-18 1997-09-17 $7700.00 Window Closed / Lapsed

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