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US4303626A Expired / Lapsed US ⏱️ 0.0 years remaining

Crystalline zeolite powder of type A (V)

Assignee: Evonik Operations GmbH
•
Filing: 1977-10-27
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Granted: 1981-12-01
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Expires: 1997-10-27
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Abstract

Abstract There are produced crystalline zeolite powders of Type A with the composition 1.0±0.2 M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5 SiO.sub.2 ·y H 2 O where M is a metal cation, n is its valence and y has a value up to 6 with 50 weight % of the particles not over 6.2μ and with a particle spectrum: ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 10 to 60 <5 25 to 95 <10 80 to 99 <15 92 to 100 ______________________________________ by hydrothermally crystallizing a SiO 2 , Al 2 O 3 , Na 2 O and water containing alkali aluminate, water, silicate synthesis mixture with an optional tempering step wherein in a given case during the crystallization or tempering step instead of stirring shearing forces are employed. The process comprises providing an aqueous alkali aluminate liquor having a temperature of 50° to 90° C. and containing 0.1 to 100 grams of Al 2 O 3 /l and 1 to 200 grams of Na 2 O/l, feeding in with stirring an alkali silicate solution, to the turbid reaction mixture having the composition SiO 2 /Al 2 O 3 =2 to 50:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/NaO=4 to 300:1, adding with stirring in two steps an aqueous sodium aluminate which contains 10 to 200 grams/l ot Al 2 O 3 and 10 to 250 grams/l of Na 2 O and having a temperature of 10° to 100° C. and allowing the thus obtained synthesis mixture to crystallize at a temperature within between 20°and 175° inside at least 15 minutes.

Inventors

  • 👤 Hans Strack
  • 👤 Wolfgang Roebke
  • 👤 Dieter Kneitel
  • 👤 Ehrfried Parr

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-07 22:01
CPC Classifications
C; C11; C11D; C11D3/00; C11D3/02; C11D3/12; C11D3/124; C11D3/1246; C11D3/128; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2815

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 279 words
A process of preparing a crystalline zeolite powder of Type A with the composition: 1.0±0.2 M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5SiO.sub.2 ·y H.sub.2 O where M is a sodium cation, n is its valence and y has a value up to 6 with 50 weight % of the particles not over 6.2μ and with a particle spectrum ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 10 to 60 <5 25 to 95 <10 80 to 99 <15 92 to 100 ______________________________________ comprising hydrothermally crystallizing a SiO 2 , Al 2 O 3 , M 2 O and water containing alkali aluminate, water, alkali silicate synthesis mixture where M is sodium, said process including the steps of providing an aqueous sodium aluminate liquor having a temperature of 50° to 90° C. and containing 0.1 to 100 grams of Al 2 O 3 /l and 1 to 200 grams of Na 2 O/l, feeding in with stirring sodium silicate solution containing 50 to 150 grams of Na 2 O/l and 200 grams to 450 grams of SiO 2 /l to form a turbid reaction mixture having the composition SiO 2 /Al 2 O 3 =2 to 50:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/Na 2 O=4 to 300:1, adding with stirring in two steps, with the second step being at a higher rate, an aqueous sodium aluminate which contains 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O and having a temperature of 10° to 100° C. and allowing the thus obtained synthesis mixture to crystallize at a temperature within between 20° and 175° C. for at least 15 minutes.
Claim 2
Dependent Claim 279 words
A process of preparing a crystalline zeolite powder of Type A with the composition: 1.0±0.2 M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5SiO.sub.2 ·y H.sub.2 O where M is a sodium cation, n is its valence and y has a value up to 6 with 50 weight % of the particles not over 6.2μ and with a particle spectrum ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 10 to 60 <5 25 to 95 <10 80 to 99 <15 92 to 100 ______________________________________ comprising hydrothermally crystallizing a SiO 2 , Al 2 O 3 , M 2 O and water containing alkali aluminate, water, alkali silicate synthesis mixture where M is sodium, said process including the steps of providing an aqueous sodium aluminate liquor having a temperature of 50° to 90° C. and containing 0.1 to 100 grams of Al 2 O 3 /l and 1 to 200 grams of Na 2 O/l, feeding in with stirring sodium silicate solution containing 50 to 150 grams of Na 2 O/l and 200 grams to 450 grams of SiO 2 /l to form a turbid reaction mixture having the composition SiO 2 /Al 2 O 3 =2 to 50:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/Na 2 O=4 to 300:1, adding with stirring in two steps, with the second step being at a higher rate, an aqueous sodium aluminate which contains 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O and having a temperature of 10° to 100° C. and allowing the thus obtained synthesis mixture to crystallize at a temperature within between 20° and 175° C. for at least 15 minutes.
Claim 3
Dependent Claim 31 words
A process according to claim 1 wherein the speed of addition of the added sodium aluminate in the second step is 2 to 10 times higher than in the first step.
Claim 4
Dependent Claim 13 words
A process according to claim 2 including a tempering step after the crystallization.
Claim 5
Dependent Claim 44 words
A process according to claim 2 wherein 10% of the aqueous sodium aluminate is added in the first step and 90% is added in the second step, the rate of addition in the second step being 2 11/35 times that in the first step.
Claim 6
Dependent Claim 26 words
A process according to claim 2 wherein a tempering step at 85° to 105° C. for 0.2 to 6 hours is carried out after the crystallization.
Claim 7
Dependent Claim 17 words
A process according to claim 5 wherein the crystallization is carried out at 90° to 100° C.
Claim 8
Dependent Claim 17 words
A process according to claim 14 wherein the crystallization is carried out at 90° to 100° C.
Claim 9
Dependent Claim 149 words
A process according to claim 2 wherein there are initially present at a temperature of 70° C. in the tank 500 liters of aqueous sodium aluminate containing 77 grams/l of Na 2 O and 6 grams/l of Al 2 O 3 , there is fed in at 20° C. within 20 minutes 300 liters of waterglass containing 7.4% Na 2 O and 25.5% SiO 2 to form a turbid solution having a temperature of 60° C. and the aqueous sodium aluminate is added to the synthesis mixture in two steps with 100 liters having a temperature of 70° C. being added in 18 minutes and then a further 900 liters of the same aqueous sodium aluminate solution having a temperature of 85° C. being added in 70 minutes, the added aqueous sodium aluminate containing 161 grams/l of Na 2 O and 105 grams/l of Al 2 O 3 .
Claim 10
Dependent Claim 13 words
A process according to claim 2 consisting essentially of the steps set forth.

References Cited (Backward Citations)

US2882243A Cited
US3058805A Cited
DE2412837A1 Cited
US3985669A Cited
US4073867A Cited
US4041135A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-11-30 1985-06-01 1985-12-01 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-11-30 1989-06-01 1989-12-01 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-11-30 1993-06-01 1993-12-01 $7700.00 Window Closed / Lapsed

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