WO1996004359A1 - Granulation in a fluidised bed - Google Patents
Granulation in a fluidised bed Download PDFInfo
- Publication number
- WO1996004359A1 WO1996004359A1 PCT/EP1995/002935 EP9502935W WO9604359A1 WO 1996004359 A1 WO1996004359 A1 WO 1996004359A1 EP 9502935 W EP9502935 W EP 9502935W WO 9604359 A1 WO9604359 A1 WO 9604359A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- acid
- process according
- precursor
- detergent composition
- bulk density
- Prior art date
Links
- 238000005469 granulation Methods 0.000 title description 4
- 230000003179 granulation Effects 0.000 title description 4
- 239000003599 detergent Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 21
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 230000000694 effects Effects 0.000 claims abstract description 9
- 239000011236 particulate material Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 19
- 239000003945 anionic surfactant Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005243 fluidization Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 229910021532 Calcite Inorganic materials 0.000 claims description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims description 2
- 239000011147 inorganic material Substances 0.000 claims description 2
- 239000012705 liquid precursor Substances 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 230000000063 preceeding effect Effects 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 description 11
- 235000017550 sodium carbonate Nutrition 0.000 description 11
- 239000004094 surface-active agent Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000000945 filler Substances 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 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 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 235000020030 perry Nutrition 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- PVGBHEUCHKGFQP-UHFFFAOYSA-N sodium;n-[5-amino-2-(4-aminophenyl)sulfonylphenyl]sulfonylacetamide Chemical compound [Na+].CC(=O)NS(=O)(=O)C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 PVGBHEUCHKGFQP-UHFFFAOYSA-N 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- 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
- C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
Definitions
- the present invention relates to a detergent composition having a low bulk density (BD) and a process for its production by dry neutralisation and further envisages the use of a fluidised bed for manufacture of such detergent compositions.
- BD bulk density
- Henkel 4304062 describes the production of a cleaning active surfactant granulate in which an anionic surfactant in acid form is neutralized with an aqueous alkali solution under high gas pressure in a granulation and drying chamber. In this process the drying of a non-surfactant liquid component by using hot air is an essential step.
- East German Patent No. 140 987 discloses a continuous process for the production of granular washing and cleaning compositions, wherein liquid components such as nonionic surfactants or the acid precursors of anionic surfactants are sprayed onto a powdered builder material, especially sodium tripolphosphate (STPP) having a high phase II content to obtain a product with bulk density ranging from 530 - 580 g/L.
- STPP sodium tripolphosphate
- the process according to the said East German Patent is restricted to the use of STPP having a high phase II content.
- GB1404317 discloses the preparation of a detergent powder of low or moderate bulk density by a dry neutralization process. Sulphonic acid is mixed with an excess of soda ash in the presence of sufficient water to initiate the neutralization reaction but not enough to wet the resulted product which is in the form of a free-flowing powder.
- the process is carried out in a mixing apparatus, for example a ribbon blender, planetary mixer or air transfer mixer.
- a mixing apparatus the particulate detergent material is subjected to compressive forces which may lead to an increase in bulk density.
- a process for the production of a " detergent composition having a low bulk density which comprises contacting an acid precursor of an anionic surfactant with a neutralizing agent in a fluidised bed to effect- neutralisation of the precursor whereby the detergent composition is obtained.
- the invention provides in a second aspect, a process for the production of a particulate detergent composition having a low bulk density which comprises feeding a particulate material comprising a neutralising agent and optionally a detergency builder in a fluidisation zone, fluidising the material, contacting a liquid precursor of an anionic surfactant with the fluidised material to effect at least partial, and preferably substantially complete, neutralisation of the acid precursor and to effect the formation of detergent particles comprising the neutralised precursor acid.
- the fluidisation zone is provided by means of a fluid bed.
- a process for the production of a particulate detergent composition having a low bulk density which comprises:-
- introducing a particulate material comprising a builder and a neutralizing agent into a fluidised bed ii. introducing linear alkyl benzene sulphonate (LAS) acid into the said bed over a sufficient time to effect at least partial neutralization of the acid and to attain the required properties of the powder.
- LAS linear alkyl benzene sulphonate
- the invention also provides a detergent composition obtainable by a process as defined in the claims.
- the process may be carried out in either batch or continuous mode of operation as desired.
- the term "detergent composition” as used herein includes a detergent material which may be mixed with other conventional materials for example bleaches and enzymes to produce a fully formulated product and also a detergent component, often referred to as an adjunct, which may be treated further to produce a detergent material which may then be mixed with other materials as desired.
- the process envisages dry neutralization of the acid precursor of an anionic surfactant with a neutralising agent by fluidisation of the neutralising agent; preferably the process is carried out in a fluidised bed.
- the process of dry neutralisation refers to at least partial and preferably substantially complete neutralisation of the acid precursor while the mixture remains in particulate form.
- addition of the acid precursor is controlled so that it does not accumulate in the unneutralised form in the detergent composition.
- the neutralising agent is suitably particulate and comprises an alkaline inorganic material, preferably an alkaline salt.
- Suitable materials include alkali metal carbonates and bicarbonates for example sodium salts thereof.
- the neutralising agent is suitably present at a level sufficient to neutralise fully the acid precursor. If desired a stoichiometric excess of neutralising agent may be employed to ensure complete neutralisation or to provide an alternative function, for example building, in the case of sodium carbonate.
- anionic surfactants or nonionic, cationic, zwitterionic, amphoteric or semipolar surfactants and mixtures thereof may be added at a suitable time.
- Suitable surfactants include those generally described in "Surface active agents and detgents " Vol I by Schwartz and Perry.
- soap derived from saturated or unsaturated fatty acids having C 12 to C 15 carbon atoms may also be present as an anionic surfactant.
- the detergent active is suitably present at a level of 5 to 40%, preferably 12 to 30% by weight of the detergent composition.
- the detergent composition suitably contains a detergency builder.
- the builder may be introduced with the neutralising agent and/or added subsequently as desired.
- the builder is introduced with the neutralising agent .
- Any conventional builder may be employed; suitable builders include sodium carbonate, zeolite, sodium tripolphosphate (STPP) sodium citrate and/or high surface area calcite.
- suitable builders include sodium carbonate, zeolite, sodium tripolphosphate (STPP) sodium citrate and/or high surface area calcite.
- STPP sodium tripolphosphate
- the builder can also consist of one of the above singularly or in combination with other builders.
- the builder and neutralising agent may be the same material, for example sodium carbonate, in which case sufficient material will be employed for both functions.
- the builder is suitably present at a level of 15 to 65% and preferably 15 to 50% by weight of the detergent composition.
- Detergent powder obtained by the present invention suitably has a low bulk density in the range 350 to 650 g/1, or 450 to 650g/l, for example, in the proximity of 500 g/L and is thus comparable to a bulk density obtained by the method of spray drying.
- a flow aid is incorporated into the composition.
- the flow aid may be mixed with the neutralising agent and, if present, builder prior to or subsequent to partial or complete addition of the acid precursor. It is especially preferred that the flow aid be added prior to or after partial introduction of the acid precursor as a significant reduction in the bulk density of the final powder may be achieved.
- the flow aid is suitably present in an amount of 0.1 to 15% by weight of the detergent composition and more preferably in an amount of 0.5 to 5%.
- Suitable flow aids include crystaline or amorphous alkali metal silicate, calcite, diatomaceous earth, silica, for example precipitated silica, magnesium sulphate, and calcium carbonate, for example precipitated calcium carbonate. Mixtures of these materials may be employed as desired.
- the flow aid is Dicamol.
- the composition may also comprise a particulate filler which suitably comprises an inorganic salt, for example sodium sulphate and sodium chloride.
- the filler may be present at a level of 5 to 50% by weight of the composition.
- the detergent composition produced according to the invention suitably comprises the detergent active and builder and optionally one or more of a flow aid, a filler and other minor ingredients such as colour, perfum, fluorescers, bleaches, enzymes.
- the particulate material (s) have a particle size distribution such that not more than 5% by weight of the particles have a particle size greater than 250 ⁇ . It is also preferred that at least 30% by weight of the particles have a particle size below 75 ⁇ .
- the particulate material (s) has an average particle size below 200 ⁇ to provide detergent powders having a particularly desired low bulk density.
- a controlled amount of water may be added to facilitate neutralisation.
- the water may be added in amounts of 0.5 to 2% by weight of the final detergents composition. Any such water is suitably prior to or together or alternating with the addition of the acid precursor.
- the particulate material is introduced into a fluidised bed and the required amount of LAS acid is then introduced preferably by spraying onto the said material and preferably from the top.
- the flow aid maybe introduced with the starting material. However, it is preferred that the flow aid be added after part introduction of part of the LAS acid to obtain a lower bulk density.
- the fluid bed is suitably operated at a temperature of ambient to 60°C.
- the air flow is sufficient to cause fluidisation and is preferably in the range 0.6 to 1 ins "1 .
- Fluidisation of the solid material is an essential feature of the present invention as this facilitates neutralisation and granulation whilst keeping the particles apart. This is to be contrasted with mixing processes in which the particles, are intentionally contacted and compressed, which may lead to higher bulk density powder and poorer powder properties.
- EXAMPLES 1 to 19 A powdered builder/inorganic alkaline material (in Examples 1 to 4, sodium carbonate performed both functions) and a filler was introduced into a fluid bed and was fluidised by operating at a superficial air velocity above the minimum fluidisation velocity. The temperature in the fluid bed was from ambient to 60°C. Linear alkyl benzene sulphonic acid (LAS acid) was sprayed onto the powdered mix in the fluid bed.
- LAS acid Linear alkyl benzene sulphonic acid
- Examples 1 to 3 illustrate the effect of incorporation a flow aid (in this case Dicamol) to the composition at different points in the process.
- a flow aid in this case Dicamol
- Example 1 the flow aid was not added to the material.
- Example 2 the flow aid was added to the starting material prior to the introduction of LAS acid.
- Example 3 the flow aid was added after introduction of 50% of the LAS acid.
- Example 4 illustrates the benefits obtained in employing a fine grade of particulate material. The results are shown below in Table 1.
- Examples 2 and 3 illustrate that a significant reduction in bulk density may be achieved by addition of the flow aid either prior to or subsequent to introduction of part of the LAS acid.
- Examples 5 to 19, as detailed below in Tables 3 to 5 were prepared according to the process described for Examples 1 to 4 and various raw materials having a different particle size distribution were employed. Table 2 summarises the size distribution of the various materials.
- Soda ash % 22.0 20.0 22.0 22.0 20.0 20.0
- Fine salt % - 30.0 - - 16.0 15.0
- Tables 3 and 4 show the results for STPP built powders containing active in the range of 17 to 31%.
- the soda ash and STPP had a similar particle size distribution as shown in Table 2 and formulations based on such builder systems resulted in products with bulk density close to 500 g/L.
- Table 5 shows powders based on various builder systems, i.e. STPP, soda ash and HSA calcite. Both the soda ash and STPP built formulations resulted in powders with BD of about 500 g/1 whereas formulations based on HSA calcites resulted in powders with bulk density lower than 500 g/L.
- Example 19 relates to a mixed active system containing 13% LAS AD and 4% soap and resulted in powder with bulk density of 500 g/L.
Landscapes
- Chemical & Material Sciences (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)
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CZ1997305A CZ289884B6 (cs) | 1994-08-05 | 1995-07-24 | Způsob výroby pracího prostředku |
HU9700357A HU222907B1 (hu) | 1994-08-05 | 1995-07-24 | Szemcsés mosószer és eljárás előállítására örvényágyas granulálással |
BR9508505A BR9508505A (pt) | 1994-08-05 | 1995-07-24 | Processo para a produção de uma composição detergente e composição detergente ou seu componente |
PL95318548A PL181161B1 (pl) | 1994-08-05 | 1995-07-24 | Sposób wytwarzania rozdrobnionej kompozycji detergentowej |
AU31656/95A AU702808B2 (en) | 1994-08-05 | 1995-07-24 | Granulation in a fluidised bed |
SK145-97A SK282576B6 (sk) | 1994-08-05 | 1995-07-24 | Spôsob výroby časticovej detergentnej zmesi |
EP95927721A EP0775193A1 (en) | 1994-08-05 | 1995-07-24 | Granulation in a fluidised bed |
MXPA/A/1997/000863A MXPA97000863A (en) | 1994-08-05 | 1997-02-03 | Granulation in a fluidized bed |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9415904A GB9415904D0 (en) | 1994-08-05 | 1994-08-05 | Process for the production of detergent composition |
GB9415904.3 | 1994-08-05 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1996004359A1 true WO1996004359A1 (en) | 1996-02-15 |
Family
ID=10759488
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP1995/002935 WO1996004359A1 (en) | 1994-08-05 | 1995-07-24 | Granulation in a fluidised bed |
Country Status (13)
Country | Link |
---|---|
EP (1) | EP0775193A1 (cs) |
CN (1) | CN1115403C (cs) |
AU (1) | AU702808B2 (cs) |
BR (1) | BR9508505A (cs) |
CA (1) | CA2195313A1 (cs) |
CZ (1) | CZ289884B6 (cs) |
GB (1) | GB9415904D0 (cs) |
HU (1) | HU222907B1 (cs) |
PL (1) | PL181161B1 (cs) |
SK (1) | SK282576B6 (cs) |
TW (1) | TW380161B (cs) |
WO (1) | WO1996004359A1 (cs) |
ZA (1) | ZA956415B (cs) |
Cited By (28)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1998058048A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
WO1998058046A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
WO1998058047A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
WO1999000475A1 (en) * | 1997-06-27 | 1999-01-07 | Unilever Plc | Production of detergent granulates |
WO1999003964A1 (en) * | 1997-07-14 | 1999-01-28 | The Procter & Gamble Company | Process for making a low density detergent composition by controlled agglomeration in a fluid bed dryer |
WO1999003967A1 (en) * | 1997-07-14 | 1999-01-28 | The Procter & Gamble Company | Process for making a low density detergent composition by controlling agglomeration via particle size |
WO2000032738A1 (de) * | 1998-12-01 | 2000-06-08 | Henkel Kommanditgesellschaft Auf Aktien | Granulationsverfahren |
US6077820A (en) * | 1995-12-20 | 2000-06-20 | Lever Brothers Company Division Of Conopco, Inc. | Process for preparing a granular detergent |
US6121229A (en) * | 1996-10-04 | 2000-09-19 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6136777A (en) * | 1996-10-04 | 2000-10-24 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6143711A (en) * | 1996-10-04 | 2000-11-07 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6150323A (en) * | 1996-10-04 | 2000-11-21 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6172034B1 (en) | 1996-10-04 | 2001-01-09 | The Procter & Gamble | Process for making a detergent composition by non-tower process |
US6211137B1 (en) | 1996-10-04 | 2001-04-03 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6211138B1 (en) | 1996-10-04 | 2001-04-03 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6362154B1 (en) | 1998-12-23 | 2002-03-26 | Henkel Kommanditgesellschaft Auf Aktien | Multiphase cleaning composition containing naphthalene sulfonic acid/formaldehyde condensate |
US6369015B1 (en) | 1998-11-20 | 2002-04-09 | Unilever Home & Personal Care, Usa Division Of Conopco, Inc. | Particulate laundry detergent compositions containing anionic surfactant granules |
US6391844B1 (en) | 1996-10-04 | 2002-05-21 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6423679B1 (en) | 1997-07-15 | 2002-07-23 | The Procter & Gamble Company | Process for making high-active detergent agglomerates by multi-stage surfactant paste injection |
US6432905B1 (en) | 1999-03-30 | 2002-08-13 | Unilever Home & Personal Care Usa Division Of Conopco, Inc. | Dry neutralization process for detergent powder composition |
US6440342B1 (en) | 1998-07-08 | 2002-08-27 | The Procter & Gamble Company | Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer |
WO2003016453A1 (en) * | 2001-08-13 | 2003-02-27 | Unilever Plc | Process for the production of detergent granules |
WO2003016454A1 (en) * | 2001-08-13 | 2003-02-27 | Unilever Plc | Process for the production of detergent granules |
US6555514B1 (en) | 1998-10-26 | 2003-04-29 | The Procter & Gamble Company | Processes for making granular detergent composition having improved appearance and solubility |
US6680288B1 (en) | 1999-11-22 | 2004-01-20 | Unilever Home & Personal Care Usa Division Of Conopco, Inc. | Process for preparing granular detergent compositions |
US6992055B1 (en) * | 1996-09-06 | 2006-01-31 | Kao Corporation | Process for preparing detergent compositions having high bulk density |
DE102005005499A1 (de) * | 2005-02-04 | 2006-08-17 | Henkel Kgaa | Verfahren zur Herstellung von Wasch- oder Reinigungsmitteln |
EP2123742A1 (en) | 2008-05-14 | 2009-11-25 | The Procter and Gamble Company | A solid laundry detergent composition comprising light density silicate salt |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1094383C (zh) * | 1998-09-11 | 2002-11-20 | 自贡市化工研究设计院 | 沉淀水合二氧化硅的喷雾—流化床造粒方法 |
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US3425948A (en) * | 1966-01-03 | 1969-02-04 | Wyandotte Chemicals Corp | Composition and process for light-weight surfactant products |
GB1369269A (en) * | 1971-02-01 | 1974-10-02 | Colgate Palmolive Co | Method for neutrlization of detergent acid |
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DD140987B1 (de) * | 1979-01-05 | 1982-06-30 | Manfred Mittelstrass | Kontinuierliches herstellungsverfahren granulierter wasch-und reinigungsmittel in wirbelschichtapparaten |
RO88903A2 (ro) * | 1983-11-04 | 1986-06-30 | Intreprinderea De Detergenti"Dero",Ro | Procedeu pentru fabricarea detergentilor granulati si instalatie pentru aplicarea acestuia |
US4734224A (en) * | 1986-09-15 | 1988-03-29 | The Dial Corporation | Dry neutralization process for detergent slurries |
EP0353976A1 (en) * | 1988-08-05 | 1990-02-07 | Cussons (International) Limited | Detergents |
DE4232874A1 (de) * | 1992-09-30 | 1994-03-31 | Henkel Kgaa | Verfahren zur Herstellung von Tensidgranulaten |
-
1994
- 1994-08-05 GB GB9415904A patent/GB9415904D0/en active Pending
-
1995
- 1995-07-24 CN CN95194514A patent/CN1115403C/zh not_active Expired - Fee Related
- 1995-07-24 SK SK145-97A patent/SK282576B6/sk unknown
- 1995-07-24 BR BR9508505A patent/BR9508505A/pt not_active IP Right Cessation
- 1995-07-24 CZ CZ1997305A patent/CZ289884B6/cs not_active IP Right Cessation
- 1995-07-24 EP EP95927721A patent/EP0775193A1/en not_active Withdrawn
- 1995-07-24 AU AU31656/95A patent/AU702808B2/en not_active Ceased
- 1995-07-24 HU HU9700357A patent/HU222907B1/hu not_active IP Right Cessation
- 1995-07-24 PL PL95318548A patent/PL181161B1/pl not_active IP Right Cessation
- 1995-07-24 WO PCT/EP1995/002935 patent/WO1996004359A1/en active IP Right Grant
- 1995-07-24 CA CA002195313A patent/CA2195313A1/en not_active Abandoned
- 1995-08-01 ZA ZA9506415A patent/ZA956415B/xx unknown
- 1995-08-09 TW TW084108296A patent/TW380161B/zh not_active IP Right Cessation
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Cited By (38)
Publication number | Priority date | Publication date | Assignee | Title |
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US6077820A (en) * | 1995-12-20 | 2000-06-20 | Lever Brothers Company Division Of Conopco, Inc. | Process for preparing a granular detergent |
US6992055B1 (en) * | 1996-09-06 | 2006-01-31 | Kao Corporation | Process for preparing detergent compositions having high bulk density |
US6136777A (en) * | 1996-10-04 | 2000-10-24 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6391844B1 (en) | 1996-10-04 | 2002-05-21 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6211138B1 (en) | 1996-10-04 | 2001-04-03 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6211137B1 (en) | 1996-10-04 | 2001-04-03 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6172034B1 (en) | 1996-10-04 | 2001-01-09 | The Procter & Gamble | Process for making a detergent composition by non-tower process |
US6150323A (en) * | 1996-10-04 | 2000-11-21 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6143711A (en) * | 1996-10-04 | 2000-11-07 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6121229A (en) * | 1996-10-04 | 2000-09-19 | The Procter & Gamble Company | Process for making a detergent composition by non-tower process |
US6274544B1 (en) | 1997-06-16 | 2001-08-14 | Lever Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
WO1998058047A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
WO1998058046A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
US6056905A (en) * | 1997-06-16 | 2000-05-02 | Lever Brothers Company Division Of Conopco, Inc. | Production of detergent granulates |
WO1998058048A1 (en) * | 1997-06-16 | 1998-12-23 | Unilever Plc | Production of detergent granulates |
AU743403B2 (en) * | 1997-06-16 | 2002-01-24 | Unilever Plc | Production of detergent granulates |
US6429184B1 (en) | 1997-06-16 | 2002-08-06 | Lever & Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
WO1999000475A1 (en) * | 1997-06-27 | 1999-01-07 | Unilever Plc | Production of detergent granulates |
US6133223A (en) * | 1997-06-27 | 2000-10-17 | Lever Brothers Company, Division Of Conopco, Inc. | Production of detergent granulates |
WO1999003967A1 (en) * | 1997-07-14 | 1999-01-28 | The Procter & Gamble Company | Process for making a low density detergent composition by controlling agglomeration via particle size |
WO1999003964A1 (en) * | 1997-07-14 | 1999-01-28 | The Procter & Gamble Company | Process for making a low density detergent composition by controlled agglomeration in a fluid bed dryer |
US6258773B1 (en) | 1997-07-14 | 2001-07-10 | The Procter & Gamble Company | Process for making a low density detergent composition by controlling agglomeration via particle size |
US6423679B1 (en) | 1997-07-15 | 2002-07-23 | The Procter & Gamble Company | Process for making high-active detergent agglomerates by multi-stage surfactant paste injection |
US6440342B1 (en) | 1998-07-08 | 2002-08-27 | The Procter & Gamble Company | Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer |
US6555514B1 (en) | 1998-10-26 | 2003-04-29 | The Procter & Gamble Company | Processes for making granular detergent composition having improved appearance and solubility |
US6369015B1 (en) | 1998-11-20 | 2002-04-09 | Unilever Home & Personal Care, Usa Division Of Conopco, Inc. | Particulate laundry detergent compositions containing anionic surfactant granules |
WO2000032738A1 (de) * | 1998-12-01 | 2000-06-08 | Henkel Kommanditgesellschaft Auf Aktien | Granulationsverfahren |
US6362154B1 (en) | 1998-12-23 | 2002-03-26 | Henkel Kommanditgesellschaft Auf Aktien | Multiphase cleaning composition containing naphthalene sulfonic acid/formaldehyde condensate |
US6432905B1 (en) | 1999-03-30 | 2002-08-13 | Unilever Home & Personal Care Usa Division Of Conopco, Inc. | Dry neutralization process for detergent powder composition |
US6680288B1 (en) | 1999-11-22 | 2004-01-20 | Unilever Home & Personal Care Usa Division Of Conopco, Inc. | Process for preparing granular detergent compositions |
WO2003016454A1 (en) * | 2001-08-13 | 2003-02-27 | Unilever Plc | Process for the production of detergent granules |
WO2003016453A1 (en) * | 2001-08-13 | 2003-02-27 | Unilever Plc | Process for the production of detergent granules |
DE102005005499A1 (de) * | 2005-02-04 | 2006-08-17 | Henkel Kgaa | Verfahren zur Herstellung von Wasch- oder Reinigungsmitteln |
EP2123742A1 (en) | 2008-05-14 | 2009-11-25 | The Procter and Gamble Company | A solid laundry detergent composition comprising light density silicate salt |
EP2123743A1 (en) | 2008-05-14 | 2009-11-25 | The Procter and Gamble Company | A solid laundry detergent composition comprising light density silicate salt |
EP2128235A1 (en) | 2008-05-14 | 2009-12-02 | The Procter and Gamble Company | A solid laundry detergent composition comprising light density silicate salt |
US7727947B2 (en) | 2008-05-14 | 2010-06-01 | The Procter & Gamble Company | Process for the preparation of a solid laundry detergent composition comprising light density silicate salt |
US7732394B2 (en) | 2008-05-14 | 2010-06-08 | The Procter & Gamble Company | Solid laundry detergent composition comprising light density silicate salt |
Also Published As
Publication number | Publication date |
---|---|
CN1155297A (zh) | 1997-07-23 |
BR9508505A (pt) | 1998-05-26 |
CA2195313A1 (en) | 1996-02-15 |
AU3165695A (en) | 1996-03-04 |
CZ289884B6 (cs) | 2002-04-17 |
SK282576B6 (sk) | 2002-10-08 |
HUT77715A (hu) | 1998-07-28 |
MX9700863A (es) | 1997-09-30 |
PL318548A1 (en) | 1997-06-23 |
GB9415904D0 (en) | 1994-09-28 |
HU222907B1 (hu) | 2003-12-29 |
PL181161B1 (pl) | 2001-06-29 |
ZA956415B (en) | 1997-02-03 |
CN1115403C (zh) | 2003-07-23 |
AU702808B2 (en) | 1999-03-04 |
TW380161B (en) | 2000-01-21 |
SK14597A3 (en) | 1997-07-09 |
CZ30597A3 (en) | 1997-09-17 |
EP0775193A1 (en) | 1997-05-28 |
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