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US4305916A Expired / Lapsed US ⏱️ 0.0 years remaining

Crystalline zeolite powder of type A (III)

Assignee: Evonik Operations GmbH
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Filing: 1977-10-27
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Granted: 1981-12-15
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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±0.2M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5SiO.sub.2.yH.sub.2 O where M is a metal cation, n is it valence and y has a value up to 6 with 50 weight % of the particles not over 4.3μ and with a particle spectrum: ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 18 to 38 <5 70 to 82 <10 93 to 99 <15 96 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 30° to 100° 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 an alkali silicate solution within 10 to 200 minutes to obtain a clear reaction solution having the composition SiO 2 /Al 2 O 3 =50 to 1000:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/Na 2 O=4 to 300:1, adding with stirring to the synthesis mixture 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 having a temperature of 30° to 100° C. and allowing the thus obtained synthesis mixture to crystallize at a temperature within between 20° and 175° C. in 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 2026-10-28 00:22
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; Y; Y10; Y10S; Y10S423/00; Y10S423/24

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 318 words
A process of preparing a crystalline zeolite powder of Type A with the composition 1.0±0.2M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5SiO.sub.2.yH.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 4.3μ and with a particle spectrum: ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 18 to 38 <5 70 to 82 <10 93 to 99 <15 96 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 alkali aluminate liquor having a temperature of 30° to 100° 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 sodium silicate solution containing 50 to 150 grams of Na 2 O/l and 200 to 450 grams of SiO 2 /l within 10 to 200 minutes to obtain a clear reaction solution having the composition SiO 2 /Al 2 O 3 =50 to 1000:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/Na 2 O=4 to 300:1, adding with stirring to the synthesis mixture an aqueous sodium aluminate containing 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O having a temperature of 30° to 100° C., the aqueous sodium aluminate having 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O being added to the synthesis mixture in two steps, the speed of addition in the second step being 2 to 10 time higher than in the first step, and allowing the thus obtained synthesis mixture to crystallize at a temperature between 20° and 170° C. for at least 15 minutes.
Claim 2
Dependent Claim 318 words
A process of preparing a crystalline zeolite powder of Type A with the composition 1.0±0.2M.sub.2/n O:Al.sub.2 O.sub.3 :1.85±0.5SiO.sub.2.yH.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 4.3μ and with a particle spectrum: ______________________________________ Fraction (μ) Portion (weight %) ______________________________________ <3 18 to 38 <5 70 to 82 <10 93 to 99 <15 96 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 alkali aluminate liquor having a temperature of 30° to 100° 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 sodium silicate solution containing 50 to 150 grams of Na 2 O/l and 200 to 450 grams of SiO 2 /l within 10 to 200 minutes to obtain a clear reaction solution having the composition SiO 2 /Al 2 O 3 =50 to 1000:1, Na 2 O/SiO 2 =0.2 to 20:1 and H 2 O/Na 2 O=4 to 300:1, adding with stirring to the synthesis mixture an aqueous sodium aluminate containing 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O having a temperature of 30° to 100° C., the aqueous sodium aluminate having 10 to 200 grams/l of Al 2 O 3 and 10 to 250 grams/l of Na 2 O being added to the synthesis mixture in two steps, the speed of addition in the second step being 2 to 10 time higher than in the first step, and allowing the thus obtained synthesis mixture to crystallize at a temperature between 20° and 170° C. for at least 15 minutes.
Claim 3
Dependent Claim 13 words
A process according to claim 1 including a tempering step after the crystallization.
Claim 4
Dependent Claim 43 words
A process according to claim 1 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 2.25 times that in the first step.
Claim 5
Dependent Claim 26 words
A process according to claim 1 wherein a tempering step at 85° to 105° C. for 0.2 to 6 hours is carried out after the crystallization.
Claim 6
Dependent Claim 17 words
A process according to claim 4 wherein the crystallization is carried out at 90° to 100° C.
Claim 7
Dependent Claim 17 words
A process according to claim 1 wherein the crystallization is carried out at 90° to 100° C.
Claim 8
Dependent Claim 128 words
A process according to claim 1 wherein there are initially present at 70° C. in the tank 500 liters of aqueous sodium aluminate containing 78 grams/l of Na 2 O and 5 grams/l of Al 2 O 3 , there is fed in 300 liters of waterglass containing 7.4% Na 2 O and 25.7% SiO 2 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 15 minutes and then a further 900 liters of the same aqueous sodium aluminate solution having a temperature of 70° C. being added in 60 minutes, added aqueous sodium aluminate containing 160 grams/l of Na 2 O and 100 grams/l of Al 2 O 3 .
Claim 9
Dependent Claim 13 words
A process according to claim 1 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) 1984-12-14 1985-06-15 1985-12-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-12-14 1989-06-15 1989-12-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-12-14 1993-06-15 1993-12-15 $7700.00 Window Closed / Lapsed

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