US3620979A - Process of forming free-flowing, particulate mixtures of phosphates and silicates - Google Patents
Process of forming free-flowing, particulate mixtures of phosphates and silicates Download PDFInfo
- Publication number
- US3620979A US3620979A US723907A US3620979DA US3620979A US 3620979 A US3620979 A US 3620979A US 723907 A US723907 A US 723907A US 3620979D A US3620979D A US 3620979DA US 3620979 A US3620979 A US 3620979A
- Authority
- US
- United States
- Prior art keywords
- alkali metal
- phosphate
- silicate
- mixture
- solution
- 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 - Lifetime
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 50
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims description 22
- 235000021317 phosphate Nutrition 0.000 title description 28
- 150000004760 silicates Chemical class 0.000 title description 4
- 150000003013 phosphoric acid derivatives Chemical class 0.000 title 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 34
- 239000010452 phosphate Substances 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 30
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 229910052681 coesite Inorganic materials 0.000 claims abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract 3
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract 3
- 229910052682 stishovite Inorganic materials 0.000 claims abstract 3
- 229910052905 tridymite Inorganic materials 0.000 claims abstract 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 18
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 8
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical group [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 6
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 34
- 229910000318 alkali metal phosphate Inorganic materials 0.000 abstract description 16
- 238000001704 evaporation Methods 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 18
- 239000000047 product Substances 0.000 description 15
- 239000004115 Sodium Silicate Substances 0.000 description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 14
- 229910052911 sodium silicate Inorganic materials 0.000 description 14
- 239000003599 detergent Substances 0.000 description 12
- 238000009472 formulation Methods 0.000 description 8
- 239000004615 ingredient Substances 0.000 description 6
- 239000001488 sodium phosphate Substances 0.000 description 5
- 235000011008 sodium phosphates Nutrition 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 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 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound 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 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-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
- 239000003513 alkali Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- -1 (KPO L Chemical compound 0.000 description 1
- GIXFALHDORQSOQ-UHFFFAOYSA-J 2,4,6,8-tetraoxido-1,3,5,7,2$l^{5},4$l^{5},6$l^{5},8$l^{5}-tetraoxatetraphosphocane 2,4,6,8-tetraoxide Chemical compound [O-]P1(=O)OP([O-])(=O)OP([O-])(=O)OP([O-])(=O)O1 GIXFALHDORQSOQ-UHFFFAOYSA-J 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 241001460678 Napo <wasp> Species 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000007973 cyanuric acids Chemical class 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- NUHSROFQTUXZQQ-UHFFFAOYSA-N isopentenyl diphosphate Chemical compound CC(=C)CCO[P@](O)(=O)OP(O)(O)=O NUHSROFQTUXZQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- UGTZMIPZNRIWHX-UHFFFAOYSA-K sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/30—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using agents to prevent the granules sticking together; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- 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
- C11D3/08—Silicates
Definitions
- the invention relates to producing free-flowing, strong, discrete, granular particles that contain a mixture of a hydratable phosphate and a silicate, and which dissolve rapidly and completely in water.
- a sodium phosphate e.g., sodium tripolyphosphate
- these may include anionic or nonionic synthetic surfactants, antiredeposition agents, such as sodium carboxymethylcellulose, extenders, perfumes, bleaching agents, e.g., chlorinated cyanurates, alkaline cleansers, e.g., soda ash, caustic soda, and the like.
- anionic or nonionic synthetic surfactants such as sodium carboxymethylcellulose
- extenders perfumes
- bleaching agents e.g., chlorinated cyanurates
- alkaline cleansers e.g., soda ash, caustic soda, and the like.
- the above phosphate built detergent when used in conventional dishwashers or cleansing equipment, is known to be corrosive to both the metal and enamelware it contacts.
- an alkali metal silicate normally sodium silicate
- the added alkali metal silicate also increases the alkali content of the detergent formulation, thereby improving detergency and buffering it against acid soils removed during cleansing.
- This patented duplex mixture has certain drawbacks. Initially, it can only be formed with the less alkaline silicates, i.e., SiO /Na O weight ratios of 3.22:] to 2.40:1. Further, when high silica to phosphate mole ratios, e.g., at least 1:1, are desired in the mixture for optimum corrosion inhibition, only the less alkaline (SiO /Na O of 3.22:1) silicates can be employed to obtain the patentees duplex product.
- an alkali metal silicate preferably a sodium silicate having an SiO,/Na O weight ratio of below 2411
- an alkali metal silicate preferably a sodium silicate having an SiO,/Na O weight ratio of below 2411
- a hydratable alkali metal phosphate either in a granular form (-10 to +200 mesh) or powdered form (-100 mesh) is used as one of the feed reactants.
- the granular form is preferred, particularly in a predominantly -20 +100 mesh size range.
- the hydratable phosphate may be either sodium tripolyphosphate, u r o tetrasodium pyrophosphate, Nla P O trisodium orthophosphate, Na PO sodium trimetaphosphate, (NaPO or the corresponding potassium salts, namely, potassium tetrametaphosphate, (KPO L, or potassium pyrophosphate, K P O
- the preferred embodiment is sodium tripolyphosphate which is most popularly used in detergent mixes.
- a hydratable phosphate e.g., sodium tripolyphosphate
- a agitated reaction chamber such as a Hobart mixer, rotary drum or other agitated vessel, heated to a temperature of 60 to 100 C. (preferably 60to 75 C.), and maintained in a state of constant agitation.
- an alkali metal silicate preferably a potassium or sodium silicate solution having an SiO /M O weight ratio of below 2.40:1, wherein M is either sodium or potassium.
- An especially useful sodium silicate solution is the Philadelphia Quartz Company product D-brand silicate which contains 14.7 percent Na O; 29.4 percent SiO and 55.9 percent H O.
- the silicate solution is dispersed onto the heated bed of hydratable phosphate, preferably through spray nozzles or other line distributing means at a rate that does not cause the resulting mixture to become excessively sticky.
- Water is constantly evaporated from the resulting mixture to prevent the incoming alkali metal silicate solution from causing the discrete particles of the mixture to adhere into undesirably large aggregates.
- the resulting mixture remains dry-appearing without changing its granular form and without losing its discrete, particulate character.
- a major portion of the granular product that is recovered is in the desired l0 mesh range when starting with the preferred -20 mesh, granular, hydratable phosphate. If a finer hydratable phosphate feed is used, i.e., a powdered phosphate, the resulting product will contain some undersized particles, that is, smaller than 80 mesh.
- any undersized particles are recycled back to the agitated bed of hydratable phosphate to be further processed until it is of suitable product size.
- Oversize particles, if any, can be crushed so that the desired product size, l +80 mesh, is separated, and any undersized fraction is recycled to the agitated, hydratable phosphate bed for further processing.
- a sodium silicate solution such as the D-brand silicate which contains about 55 percent water can be used as received from the manufacturer and added directly to the sodium tripolyphosphate.
- sufficient water may be added to the silicate solution to reduce the viscosity of the solution to a suitable, workable level.
- the added water permits the silicate solution to be more readily dispersed throughout the bed of hydratable phosphate.
- the addition of excessive amounts of water is undesirable because this water must be evaporated from the mixture and increases the reaction time and heat input required to prepare the final product.
- Si0 to sodium tripolyphosphate mole ratio at a level of at least 1:1 in order to provide good corrosion inhibition.
- This and higher mole ratios of silicate to sodium tripolyphosphate are sufficient to materially reduce or eliminate undue corrosion of metal equipment that contacts the present silicate-phosphate product when it is incorporated in a final detergent formulation. Examples of some sodium silicate solutions which have been found effective in the present invention are listed below:
- EXAMPLE 1 dropwise at a rate of about 0.2 gram/minute. Water was continuously evaporated from the mixture during the run. The rate of addition of the silicate solution was controlled by observing the mixture; if the discrete particles of the mixture commenced to adhere into undesirably large aggregates, the
- EXAMPLE 2 The procedure of example 1, run 1, was repeated, except that Kasil 88," a proprietary product containing 9.1 weight percent K 0, 19.9 weight percent SiO and 71 weight percent H O was used in place of the sodium silicate solution.
- Kasil 88 a proprietary product containing 9.1 weight percent K 0, 19.9 weight percent SiO and 71 weight percent H O was used in place of the sodium silicate solution.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Detergent Compositions (AREA)
- Glanulating (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US72390768A | 1968-04-24 | 1968-04-24 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3620979A true US3620979A (en) | 1971-11-16 |
Family
ID=24908197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US723907A Expired - Lifetime US3620979A (en) | 1968-04-24 | 1968-04-24 | Process of forming free-flowing, particulate mixtures of phosphates and silicates |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US3620979A (ja) |
| JP (1) | JPS4831472B1 (ja) |
| BE (1) | BE731431A (ja) |
| BR (1) | BR6908202D0 (ja) |
| CH (1) | CH533169A (ja) |
| DE (1) | DE1919093A1 (ja) |
| ES (1) | ES366406A1 (ja) |
| FR (1) | FR2006800A1 (ja) |
| GB (1) | GB1241393A (ja) |
| NL (1) | NL6906300A (ja) |
| SE (1) | SE345138B (ja) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3888781A (en) * | 1972-09-05 | 1975-06-10 | Procter & Gamble | Process for preparing a granular automatic dishwashing detergent composition |
| US3901831A (en) * | 1973-08-24 | 1975-08-26 | Monsanto Co | Method of making dense detergent granules |
| US3950275A (en) * | 1972-08-17 | 1976-04-13 | Lion Fat & Oil Co., Ltd. | Method of manufacturing granular detergents |
| US4032465A (en) * | 1975-02-03 | 1977-06-28 | Lever Brothers Company | Production of detergent compositions |
| US4043789A (en) * | 1974-03-19 | 1977-08-23 | Norsk Hydro A.S | Process for manufacturing of phosphoric acid |
| US4131558A (en) * | 1975-02-14 | 1978-12-26 | The Procter & Gamble Company | Process for preparing an orthophosphate-silicate detergent product |
| US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| US4228025A (en) * | 1979-06-29 | 1980-10-14 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| US5180515A (en) * | 1989-07-27 | 1993-01-19 | The Procter & Gamble Company | Granular detergent compositions having low levels of potassium salt to provide improved solubility |
| US5811080A (en) * | 1996-11-26 | 1998-09-22 | The Procter & Gamble Company | Process for increased flavor impact in oral care products |
| EP1624049A2 (en) * | 2003-05-15 | 2006-02-08 | Kao Corporation | A sliding property improver for use in washing |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2707280A1 (de) * | 1976-02-26 | 1977-09-01 | Colgate Palmolive Co | Verfahren zur herstellung freifliessender spruehgetrockneter teilchen aus buildersalzen |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2909490A (en) * | 1954-07-28 | 1959-10-20 | Olin Mathieson | Manufacture of duplex composition of sodium tripolyphosphate and sodium silicate solution |
| US3390093A (en) * | 1962-06-06 | 1968-06-25 | Monsanto Co | Detergent compositions containing hydrated alkali metal tripolyphosphates |
-
1968
- 1968-04-24 US US723907A patent/US3620979A/en not_active Expired - Lifetime
-
1969
- 1969-03-31 GB GB06661/69A patent/GB1241393A/en not_active Expired
- 1969-04-10 FR FR6911148A patent/FR2006800A1/fr not_active Withdrawn
- 1969-04-11 BE BE731431D patent/BE731431A/xx unknown
- 1969-04-15 DE DE19691919093 patent/DE1919093A1/de active Pending
- 1969-04-18 BR BR208202/69A patent/BR6908202D0/pt unknown
- 1969-04-22 JP JP44030826A patent/JPS4831472B1/ja active Pending
- 1969-04-23 SE SE5808/69A patent/SE345138B/xx unknown
- 1969-04-23 NL NL6906300A patent/NL6906300A/xx unknown
- 1969-04-24 ES ES366406A patent/ES366406A1/es not_active Expired
- 1969-04-24 CH CH624369A patent/CH533169A/de not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2909490A (en) * | 1954-07-28 | 1959-10-20 | Olin Mathieson | Manufacture of duplex composition of sodium tripolyphosphate and sodium silicate solution |
| US3390093A (en) * | 1962-06-06 | 1968-06-25 | Monsanto Co | Detergent compositions containing hydrated alkali metal tripolyphosphates |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3950275A (en) * | 1972-08-17 | 1976-04-13 | Lion Fat & Oil Co., Ltd. | Method of manufacturing granular detergents |
| US3888781A (en) * | 1972-09-05 | 1975-06-10 | Procter & Gamble | Process for preparing a granular automatic dishwashing detergent composition |
| US3901831A (en) * | 1973-08-24 | 1975-08-26 | Monsanto Co | Method of making dense detergent granules |
| US4043789A (en) * | 1974-03-19 | 1977-08-23 | Norsk Hydro A.S | Process for manufacturing of phosphoric acid |
| US4032465A (en) * | 1975-02-03 | 1977-06-28 | Lever Brothers Company | Production of detergent compositions |
| US4131558A (en) * | 1975-02-14 | 1978-12-26 | The Procter & Gamble Company | Process for preparing an orthophosphate-silicate detergent product |
| US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| US4228025A (en) * | 1979-06-29 | 1980-10-14 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
| US5180515A (en) * | 1989-07-27 | 1993-01-19 | The Procter & Gamble Company | Granular detergent compositions having low levels of potassium salt to provide improved solubility |
| US5811080A (en) * | 1996-11-26 | 1998-09-22 | The Procter & Gamble Company | Process for increased flavor impact in oral care products |
| EP1624049A2 (en) * | 2003-05-15 | 2006-02-08 | Kao Corporation | A sliding property improver for use in washing |
| EP1624049A4 (en) * | 2003-05-15 | 2006-06-14 | Kao Corp | IMPROVED SLIDING PROPERTY FOR USE IN WASHING |
Also Published As
| Publication number | Publication date |
|---|---|
| ES366406A1 (es) | 1971-03-16 |
| GB1241393A (en) | 1971-08-04 |
| NL6906300A (ja) | 1969-10-28 |
| BE731431A (ja) | 1969-09-15 |
| FR2006800A1 (ja) | 1970-01-02 |
| CH533169A (de) | 1973-01-31 |
| DE1919093A1 (de) | 1970-05-21 |
| BR6908202D0 (pt) | 1973-01-02 |
| JPS4831472B1 (ja) | 1973-09-29 |
| SE345138B (ja) | 1972-05-15 |
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