EP0061600A1 - Procédé de fabrication de granulés mixtes de phosphates condensés et de charges - Google Patents
Procédé de fabrication de granulés mixtes de phosphates condensés et de charges Download PDFInfo
- Publication number
- EP0061600A1 EP0061600A1 EP82101656A EP82101656A EP0061600A1 EP 0061600 A1 EP0061600 A1 EP 0061600A1 EP 82101656 A EP82101656 A EP 82101656A EP 82101656 A EP82101656 A EP 82101656A EP 0061600 A1 EP0061600 A1 EP 0061600A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- amount
- mixture
- water
- ammonium polyphosphate
- weight
- 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.)
- Granted
Links
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 40
- 235000021317 phosphate Nutrition 0.000 title claims abstract description 40
- 239000008187 granular material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 150000003013 phosphoric acid derivatives Chemical class 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims 2
- 239000000203 mixture Substances 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 26
- 239000010452 phosphate Substances 0.000 claims abstract description 26
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 21
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 21
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 7
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 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 4
- 239000001226 triphosphate Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Chemical group 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 150000001447 alkali salts Chemical class 0.000 claims 1
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 239000003599 detergent Substances 0.000 description 7
- 239000000155 melt Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- -1 For example Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 101100399296 Mus musculus Lime1 gene Proteins 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005406 washing Methods 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
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
- C11D3/062—Special methods concerning phosphates
Definitions
- the invention relates to a process for preparing mixed granulates from water-soluble condensed phosphates th of the general formula M 2 O (MPO 3) n in which M is sodium, potassium or ammonium, and n is a number between 4 and about 100, and builder salts.
- M is sodium, potassium or ammonium
- n is a number between 4 and about 100, and builder salts.
- the P 2 0 5 content of the condensed phosphates ranges from 60.4 to 69.6%.
- Na 2 CO 3 is used as the anhydrous component
- the mixture is given a high level of alkalinity, which severely limits the range of use of the mixture in the detergent sector.
- the total phosphate content is increased to an undesirable extent, so that such mixtures are not suitable for use as a component of detergent formulations with a reduced phosphate content.
- the object of the present invention is to produce mixed granules from condensed phosphates and builder salts using the smallest possible amounts of granulating aids which do not adversely affect the wash-active properties of the condensed phosphate.
- the granules produced should be free-flowing, storable and abrasion-resistant, so that they can be admixed as a detergent component to a base product produced by the hot spray process.
- alkali metal salts of nitrilotriacetic acid and / or of poly-a-hydroxyacrylic acid and / or polyacrylic acid are preferably used as builder salts, the latter having a molecular weight of about 2000 to 30,000.
- the polyphosphate of the general formula II must correspond in which n is an integer average value from 3 to 1000, in particular 10 to 1000, m is an integer up to a maximum of n + 2 and m / n is a value from 1.0 to 1.67, in particular approximately 1, corresponds.
- the amount of builder is 5 to 50 Ge, 1%, the amount of ammonium polyphosphate 0.04-0.4% by weight and the amount of water 2-9% by weight, based in each case on the amount of the condensed phosphate.
- the latter is advantageously characterized by a P 2 0 5 content of 60.4 to 69.6% by weight.
- a variant of the process according to the invention consists in that the spraying of the water or the aqueous ammonium polyphosphate solution onto the mixture provided is carried out intermittently, the interruptions taking about 2 minutes. After each spray phase, the resulting granules can optionally be powdered on the surface with powdered pentasodium triphosphate.
- abrasion-resistant, storable and non-baking mixed granules with a considerable proportion of condensed phosphates are obtained, which is surprising insofar as it was previously assumed that water would not be suitable for granulating melt phosphates or their mixtures with other substances and in use of water as a granulating aid, there would always be caking of the melt phosphate particles to form undesired larger aggregates, unless hydrated water-free salts which prevent water absorption of the melt phosphate are added to the melt phosphate.
- the present invention is not tied to such a restriction, since the degree of hydration of the other granulate components is insignificant due to the presence of the ammonium polyphosphate as a binder.
- the bulk density of the granules was 65 g / l. After storage for one week in a thin-walled plastic bag that was permeable to air humidity, only a few agglomerates had formed, which disintegrated into the individual granules due to little mechanical action.
- Example 2 25 kg of a mixture corresponding to Example 1 were placed on a rotating turntable and the mixture was again intermittently sprayed with a 4% by weight solution of ammonium polyphosphate.
- the mixture on the turntable was powdered with a total of 5 kg of a finely divided sodium tripolyphosphate after each spray phase. It had a hard granules formed, the particles than 150 / um were coarser to 85.6%.
- the ammonium polyphos The phate content of the granules was 0.1% by weight, based on the amount of melt phosphate, and the bulk density was 63o g / l.
- the abrasion resistance of the granules determined by the drum method gave a value of 69%. After storage for one week under the same conditions as in Example 1, there was still a slight tendency to form agglomerates.
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)
- Detergent Compositions (AREA)
- Glanulating (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT82101656T ATE11563T1 (de) | 1981-03-25 | 1982-03-04 | Verfahren zur herstellung von mischgranulaten aus kondensierten phosphaten und gerueststoffsalzen. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19813111617 DE3111617A1 (de) | 1981-03-25 | 1981-03-25 | Verfahren zur herstellung von mischgranulaten aus kondensierten phosphaten und gerueststoffsalzen |
| DE3111617 | 1981-03-25 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0061600A1 true EP0061600A1 (fr) | 1982-10-06 |
| EP0061600B1 EP0061600B1 (fr) | 1985-01-30 |
Family
ID=6128175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP82101656A Expired EP0061600B1 (fr) | 1981-03-25 | 1982-03-04 | Procédé de fabrication de granulés mixtes de phosphates condensés et de charges |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US4517109A (fr) |
| EP (1) | EP0061600B1 (fr) |
| AT (1) | ATE11563T1 (fr) |
| CA (1) | CA1152844A (fr) |
| DE (2) | DE3111617A1 (fr) |
| DK (1) | DK134482A (fr) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995015370A1 (fr) * | 1993-12-03 | 1995-06-08 | Monsanto Company | Nitrilotriacetate de metal alcalin granulaire |
| US5998663A (en) * | 1998-01-14 | 1999-12-07 | Solutia, Inc. | Granular alkali metal nitrilotriacetate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1102329B (de) * | 1959-10-01 | 1961-03-16 | Basf Ag | Spuelmittel zur Verhinderung von Inkrustierungen im Textilgut nach dem Waschen |
| US3354092A (en) * | 1963-01-14 | 1967-11-21 | Procter & Gamble | Ammoniated granular cleaner |
| DE1903831A1 (de) * | 1969-01-27 | 1970-09-03 | Miele & Cie Maschinenfabrik | Reinigungsmittel fuer Geschirrspuelautomaten |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2904513A (en) * | 1954-04-16 | 1959-09-15 | Monsanto Chemicals | Inorganic phosphate compositions, and methods for the preparation and utilization thereof |
| US3627686A (en) * | 1968-09-30 | 1971-12-14 | Chemed Corp | Machine dishwashing compositions containing sodium polyacrylate and nta |
| GB1384241A (en) * | 1971-02-23 | 1975-02-19 | Albright & Wilson | Manufacture of ammonium polyphosphate |
| US4077897A (en) * | 1976-02-13 | 1978-03-07 | The Procter & Gamble Company | Process for preparing detergent compositions |
| US4228025A (en) * | 1979-06-29 | 1980-10-14 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| DE3035805A1 (de) * | 1980-09-23 | 1982-05-06 | Hoechst Ag, 6000 Frankfurt | Verfahren zur herstellung von granulaten kondensierter phosphate |
-
1981
- 1981-03-25 DE DE19813111617 patent/DE3111617A1/de not_active Withdrawn
-
1982
- 1982-03-04 EP EP82101656A patent/EP0061600B1/fr not_active Expired
- 1982-03-04 AT AT82101656T patent/ATE11563T1/de not_active IP Right Cessation
- 1982-03-04 DE DE8282101656T patent/DE3262089D1/de not_active Expired
- 1982-03-24 CA CA000399296A patent/CA1152844A/fr not_active Expired
- 1982-03-24 DK DK134482A patent/DK134482A/da not_active Application Discontinuation
-
1983
- 1983-10-14 US US06/542,075 patent/US4517109A/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1102329B (de) * | 1959-10-01 | 1961-03-16 | Basf Ag | Spuelmittel zur Verhinderung von Inkrustierungen im Textilgut nach dem Waschen |
| US3354092A (en) * | 1963-01-14 | 1967-11-21 | Procter & Gamble | Ammoniated granular cleaner |
| DE1903831A1 (de) * | 1969-01-27 | 1970-09-03 | Miele & Cie Maschinenfabrik | Reinigungsmittel fuer Geschirrspuelautomaten |
Also Published As
| Publication number | Publication date |
|---|---|
| DK134482A (da) | 1982-09-26 |
| ATE11563T1 (de) | 1985-02-15 |
| US4517109A (en) | 1985-05-14 |
| EP0061600B1 (fr) | 1985-01-30 |
| CA1152844A (fr) | 1983-08-30 |
| DE3111617A1 (de) | 1982-10-07 |
| DE3262089D1 (en) | 1985-03-14 |
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