EP0061599B1 - Granulé à base de silicate d'aluminium et de métal alcalin et de triphosphate pentasodique et procédé de préparation - Google Patents
Granulé à base de silicate d'aluminium et de métal alcalin et de triphosphate pentasodique et procédé de préparation Download PDFInfo
- Publication number
- EP0061599B1 EP0061599B1 EP82101655A EP82101655A EP0061599B1 EP 0061599 B1 EP0061599 B1 EP 0061599B1 EP 82101655 A EP82101655 A EP 82101655A EP 82101655 A EP82101655 A EP 82101655A EP 0061599 B1 EP0061599 B1 EP 0061599B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- aluminosilicate
- granulate
- pentasodium triphosphate
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000008187 granular material Substances 0.000 title claims abstract description 35
- 235000019832 sodium triphosphate Nutrition 0.000 title claims abstract description 34
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 title claims abstract 3
- 229910000323 aluminium silicate Inorganic materials 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 13
- -1 alkali metal aluminium silicate Chemical class 0.000 title claims 4
- 239000005995 Aluminium silicate Substances 0.000 title 1
- 229910052783 alkali metal Inorganic materials 0.000 title 1
- 235000012211 aluminium silicate Nutrition 0.000 title 1
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 19
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 14
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 30
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 30
- 239000001226 triphosphate Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000010457 zeolite Substances 0.000 claims description 13
- 238000005507 spraying Methods 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 150000004687 hexahydrates Chemical class 0.000 claims description 4
- 241000282326 Felis catus Species 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 230000036571 hydration Effects 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 239000003599 detergent Substances 0.000 abstract description 5
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 9
- 239000003513 alkali Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- UBWXUGDQUBIEIZ-QNTYDACNSA-N nandrolone phenpropionate Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@H]4CCC(=O)C=C4CC3)CC[C@@]21C)C(=O)CCC1=CC=CC=C1 UBWXUGDQUBIEIZ-QNTYDACNSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229920000388 Polyphosphate Polymers 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000001205 polyphosphate Substances 0.000 description 3
- 235000011176 polyphosphates Nutrition 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 235000011178 triphosphate Nutrition 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
Definitions
- Alkaline alumosilicates especially crystalline or amorphous zeolites, are becoming increasingly important as detergent builders.
- these builders only reach in combination with other complexing agents for divalent cations such as. B. pentasodium triphosphate, NTPP for short, optimal washing properties.
- B. pentasodium triphosphate, NTPP for short, optimal washing properties.
- alkali alumosilicates are fine powder, there is great interest in non-dusting, free-flowing granules which contain both alkali alumosilicates and NTPP. These can then be added dry to the other detergent components without dust formation, hydrolysis of the triphosphate also being avoided.
- DE-A-2 714 604 describes a granulate consisting of ion-exchanging alkali alumosilicate, a highly polymeric phosphate with a P 2 0 s content of 64-69%, and pentasodium triphosphate.
- the high polymer phosphate is added to the granulation mixture in powder form in the form of alkali salts and in an amount of at least 5% by weight, based on the alkali alumosilicate used. The mixture is then granulated in the presence of water.
- This method has the disadvantage that the water is bound by the NTPP so quickly that it is no longer able to dissolve enough polymer phosphate for better granulation. Therefore, either larger amounts of polymer phosphate and longer vellwell times are required, or more water has to be added, which means that the granules have to be subsequently dried at 50 ° C.
- DE-A-2 756 732 describes a granulate which likewise consists of alkali alumosilicate and a partially or fully hydrated alkali polyphosphate.
- This granulate is produced by spraying water in fine mists onto the powder mixture of the granulate components, with a maximum of 10% of the total amount of water being allowed to be added per minute, since otherwise too large granulate particles are obtained in addition to a high dust content. This process therefore harbors the danger of producing granules with a very broad grain spectrum which still have to be sieved afterwards.
- DE-A-2 822 231 describes granules of hydrated pentasodium triphosphate and water-insoluble aluminosilicate ion exchange material. This is also produced by spraying water onto the powder mixture, the total amount of water used being at least that required to achieve a minimum hydrate water content of about 10% by weight in the sodium tripolyphosphate and a water content in the aluminosilicate ion exchange material of 1.8 to 13.5 mol water per mol aluminosilicate .
- the strength of the granulate particles obtained in this way can still be improved, as will be shown below with reference to the invention.
- the proportion of the partially or fully hydrated pentasodium triphosphate is 30-70% by weight and the proportion of the ammonium polyphosphate is 0.03 to 1.6% by weight. At least 10% by weight of the pentasodium triphosphate is present here tes as hexahydrate and at least 30 wt .-% of the aluminosilicate as hydrate with a maximum of 13.5 moles of water per mole of aluminosilicate.
- spraying is preferably carried out on an intimate powdery mixture of 1 to 99% by weight of an anhydrous or optionally at most 5% by weight water-containing pentasodium triphosphate and 99 to 1% by weight of a powdered, anhydrous or optionally bound water containing aluminosilicate ion exchange material of the general formula in which Kat, Me, w, x and y have the meaning given, with vigorous mixing, an aqueous 0.5-20% by weight solution in a fine mist and granulates the mixture with partial or complete hydration of the pentasodium triphosphate or Aluminum silicate exchange material.
- the powdery mixture can consist of 30 to 70% by weight of the pentasodium triphosphate and 70 to 30% by weight of the aluminosilicate, the latter, for example, a zeolite of the formula can be.
- the pentasodium triphosphate is present as hexahydrate and at least 30% by weight of the aluminosilicate is present as a hydrate with at most 13.5 mol of water per mol of aluminosilicate in the finished granulate.
- the mixture is generally sprayed with an aqueous 1-10% by weight solution of ammonium polyphosphate.
- Products of the aforementioned formula composition are to be used as the aluminosilicate ion exchange material.
- Zeolites such as e.g. Zeolite A. Because of their use as detergent builders, they are in very fine-particle form, for example with an average particle diameter of 3-5 ⁇ m.
- the P 2 0 5 content of the ammonium polyphosphate used for the granulation is more than 69%, polyphosphates with a P 2 0 5 content of over 71% being preferred.
- the process according to the invention can be carried out, for example, by first mixing the pentasodium triphosphate with the aluminosilicate material in a mixer and then spraying the aqueous ammonium polyphosphate solution onto the mixture via a nozzle.
- the spraying can also be carried out, for example, in a rotary tube or on a granulating plate onto the premixed material. It is important to ensure that no more granulating liquid is sprayed on than is necessary for the complete hydration of the sodium triphosphate contained in the mixture.
- a granulate produced in this way is not dusty, abrasion-resistant and stable in storage. It meets the requirements for further processing in detergents by dry admixing.
- Example 2 The procedure was as in Example 1, but using a 4% aqueous APP solution.
- the mixed granules obtained from sodium triphosphate and zeolite had the following properties:
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Detergent Compositions (AREA)
Claims (9)
1. Granulé contenant un triphosphate pentasodique partiellement ou complètement hydraté ainsi qu'un aluminosilicate échangeur d'ions insoluble dans l'eau de formule générale (II)
dans laquelle cat est un cation de valence w remplaçable par le calcium, x est un nombre de 0,7-1,5, Me représente le bore ou l'aluminium y est un nombre de 0,8-6 et z est un nombre de 1,8-13,5, caractérisé en ce qu'il présente
a) une granulométrie de 0,2-2 mm; et contient,
b) 2-95% en poids de triphosphate pentasodique,
c) moins de 3% en poids d'un polyphosphate d'ammonium de formule générale (1)
dans laquelle n représente un entier.d'une valeur moyenne de 100-1000, m est un nombre entier égal au maximum à n+2 et m/n est une valeur d'environ 1; et, comme complément,
d) l'aluminosilicate échangeur d'ions mentionné.
2. Granulé selon la revendication 1, caractérisé en ce qu'il contient 30-70% en poids de triphosphate pentasodique partiellement ou complètement hydraté.
3. Granulé selon la revendication 1 ou 2, caractérisé en ce qu'il contient 0,03-1,6% en poids de polyphosphate d'ammonium.
4. Granulé selon les revendications 1 à 3, caractérisé en ce qu'il contient au moins 10% en poids du triphosphate pentasodique sous forme d'hexahydrate et au moins 30% de l'aluminosilicate sous forme d'hydrate ayant au plus 13,5 mol d'eau par mol d'aluminosilicate.
5. Procédé de préparation des granulés selon l'une des revendications 1 à 4, caractérisé en ce que l'on projette sous agitation énergique un fin brouillard d'une solution aqueuse à 0,5-20% en poids d'un polyphosphate d'ammonium de formule générale (1) sur un mélange pulvérulent intime de 1-99% en poids d'un triphosphate pentasodique anhydre ou contenant éventuellement au plus 5% en poids d'eau et de 99-1% en poids d'un aluminosilicate échangeur d'ions pulvérulent, anhydre ou contenant éventuellement de l'eau liée, répondant à la formule générale
dans laquelle cat, Me, w, x et y ont les significations déjà données, et on granule le mélange avec hydratation partielle ou complète du triphosphate pentasodique ou de l'aluminosilicate échangeur d'ions.
6. Procédé selon la revendication 5, caractérisé en ce que le mélange pulvérulent est constitué par 30-70% en poids de triphosphate pentasodique et 70-30% en poids d'aluminosilicate.
7. Procédé selon la revendication 5 ou 6, caractérisé en ce que l'aluminosilicate échangeur d'ions est une zéolite de formule
8. Procédé selon les revendications 5 à 7, caractérisé en ce que l'on utilise pour la granulation une quantité d'eau nécessaire pour avoir dans le granulé fini au moins 10% en poids du triphosphate pentasodique sous forme de l'hexahydrate et au moins 30% en poids de l'aluminosilicate sous forme de l'hydrate contenant au plus 13,5 moles d'eau par mole d'aluminosilicate.
9. Procédé selon l'une des revendications 5 à 8, caractérisé en ce que l'on projette sur le mélange une solution aqueuse à 1-10% en poids de polyphosphate d'ammonium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT82101655T ATE11792T1 (de) | 1981-03-21 | 1982-03-04 | Granulat aus alkalialumosilicat und pentanatriumtriphosphat sowie verfahren zu dessen herstellung. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3111236 | 1981-03-21 | ||
| DE3111236A DE3111236A1 (de) | 1981-03-21 | 1981-03-21 | Granulat aus alkalialuminiumsilikat und pentanatrium-triphosphat sowie verfahren zu dessen herstellung |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0061599A1 EP0061599A1 (fr) | 1982-10-06 |
| EP0061599B1 true EP0061599B1 (fr) | 1985-02-13 |
| EP0061599B2 EP0061599B2 (fr) | 1988-07-06 |
Family
ID=6127993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP82101655A Expired EP0061599B2 (fr) | 1981-03-21 | 1982-03-04 | Granulé à base de silicate d'aluminium et de métal alcalin et de triphosphate pentasodique et procédé de préparation |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US4386024A (fr) |
| EP (1) | EP0061599B2 (fr) |
| AT (1) | ATE11792T1 (fr) |
| CA (1) | CA1161416A (fr) |
| DE (2) | DE3111236A1 (fr) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3208138A1 (de) * | 1982-03-06 | 1983-09-08 | Hoechst Ag, 6230 Frankfurt | Cogranulat aus alkalisilikat und alkalipolyphosphat sowie verfahren zur herstellung des granulates |
| US4711748A (en) * | 1985-12-06 | 1987-12-08 | Lever Brothers Company | Preparation of bleach catalyst aggregates of manganese cation impregnated aluminosilicates by high velocity granulation |
| US4655782A (en) * | 1985-12-06 | 1987-04-07 | Lever Brothers Company | Bleach composition of detergent base powder and agglomerated manganese-alluminosilicate catalyst having phosphate salt distributed therebetween |
| DE4009082A1 (de) * | 1990-03-21 | 1991-09-26 | Aquamot Ag | Verfahren zur reinigung von industriellen, landwirtschaftlichen oder privaten abwaessern von ihren verunreinigungen an ammoniumverbindungen |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2801978A (en) * | 1956-11-02 | 1957-08-06 | B T Babbitt Inc | Ammonia-containing detergents |
| US4014806A (en) * | 1973-12-07 | 1977-03-29 | David Connor | Novel organopolyphosphates in aqueous cleaning compositions |
| US4248911A (en) * | 1976-12-02 | 1981-02-03 | Colgate-Palmolive Company | Concentrated heavy duty particulate laundry detergent |
| DE2714604C3 (de) * | 1977-04-01 | 1985-04-25 | Joh. A. Benckiser Gmbh, 6700 Ludwigshafen | Granulat auf Basis von polymerem Phosphat und ionenaustauschendem Alkalialumosilikat |
| DE2744773C3 (de) * | 1977-10-05 | 1986-08-21 | Joh. A. Benckiser Gmbh, 6700 Ludwigshafen | Granulat auf Basis von polymerem Phosphat und ionenaustauschendem Alkalialumosilikat |
| DE2751354A1 (de) * | 1977-11-17 | 1979-05-23 | Hoechst Ag | Verfahren zur herstellung von gemischen aus kristallinem zeolith und natriumtriphosphat |
| DE2822231A1 (de) * | 1978-05-22 | 1979-11-29 | Hoechst Ag | Granulat aus hydratisiertem natriumtripolyphosphat und wasserunloeslichem alumosilicationenaustauschmaterial |
| DE2829165A1 (de) * | 1978-07-03 | 1980-01-17 | Henkel Kgaa | Verfahren zur herstellung von alumosilikat-granulat |
-
1981
- 1981-03-21 DE DE3111236A patent/DE3111236A1/de not_active Withdrawn
-
1982
- 1982-03-04 DE DE8282101655T patent/DE3262256D1/de not_active Expired
- 1982-03-04 EP EP82101655A patent/EP0061599B2/fr not_active Expired
- 1982-03-04 AT AT82101655T patent/ATE11792T1/de not_active IP Right Cessation
- 1982-03-10 CA CA000398044A patent/CA1161416A/fr not_active Expired
- 1982-03-15 US US06/358,388 patent/US4386024A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| ATE11792T1 (de) | 1985-02-15 |
| EP0061599B2 (fr) | 1988-07-06 |
| DE3111236A1 (de) | 1982-09-30 |
| DE3262256D1 (en) | 1985-03-28 |
| CA1161416A (fr) | 1984-01-31 |
| US4386024A (en) | 1983-05-31 |
| EP0061599A1 (fr) | 1982-10-06 |
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