WO1999032599A1 - Procede de production de particules - Google Patents
Procede de production de particules Download PDFInfo
- Publication number
- WO1999032599A1 WO1999032599A1 PCT/GB1998/003791 GB9803791W WO9932599A1 WO 1999032599 A1 WO1999032599 A1 WO 1999032599A1 GB 9803791 W GB9803791 W GB 9803791W WO 9932599 A1 WO9932599 A1 WO 9932599A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- anionic surfactant
- surfactant
- builder
- extruder
- extrusion
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 73
- 238000001125 extrusion Methods 0.000 claims abstract description 46
- 239000003599 detergent Substances 0.000 claims abstract description 20
- 125000000129 anionic group Chemical group 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 57
- 239000000463 material Substances 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 229910001868 water Inorganic materials 0.000 claims description 32
- 239000002736 nonionic surfactant Substances 0.000 claims description 23
- 238000009472 formulation Methods 0.000 claims description 19
- 239000002671 adjuvant Substances 0.000 claims description 14
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 13
- -1 alkali metal salt Chemical class 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 claims description 7
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 125000002947 alkylene group Chemical group 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 239000007859 condensation product Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 35
- 238000001035 drying Methods 0.000 description 19
- 230000008569 process Effects 0.000 description 19
- 239000000047 product Substances 0.000 description 19
- 238000002156 mixing Methods 0.000 description 15
- 239000007787 solid Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 238000007792 addition Methods 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 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 8
- 125000000217 alkyl group Chemical group 0.000 description 7
- 239000008187 granular material Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 150000001340 alkali metals Chemical class 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- 239000010457 zeolite Substances 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 description 3
- 239000003752 hydrotrope Substances 0.000 description 3
- 150000003839 salts Chemical group 0.000 description 3
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 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
- 239000000654 additive Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 235000012149 noodles Nutrition 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002190 fatty acyls Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000000344 soap 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
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 235000018341 sodium sesquicarbonate Nutrition 0.000 description 1
- 229910000031 sodium sesquicarbonate Inorganic materials 0.000 description 1
- 235000019794 sodium silicate Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
- 238000011144 upstream manufacturing 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
- 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
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
Definitions
- This invention relates to a method of manufacturing surfactant particles comprising an anionic surfactant.
- Some processes seek to overcome the problems by using pre-dried surfactant, typically produced by spray-drying.
- a small amount of liquid is added to act as a binding agent.
- a further limitation of conventional agglomeration systems is that they tend to give a granule of lower bulk density than the feed materials, due to the inclusion of air in the granules.
- EP-A-349200 describes a process for making dense, concentrated detergent granules from a surfactant paste using fine dispersion cold granulation.
- a preferred temperature range is from about -30°C to about 0°C.
- the surfactant paste can be introduced into the mixer at an initial temperature in the range about 5-70°C, especially about 20-30°C; it is stated that a temperature greater than about 70°C can lead to poor initial mixing due to increased product stickiness.
- the paste is preferably cooled to the granulation temperature by addition of dry ice.
- EP-A-340966 describes a process of making a high density particulate detergent composition, involving turbodrying a mixture of an anionic surfactant, water and bentonite.
- turbodryer subjects the mixture to centrifugal and axial forces while it is being dried.
- US-A-5290496 describes a process for manufacturing granules by a process in which detergent components are mixed together to form a free-flowing premix, for charging a homogenizing unit, for example a twin-screw kneader in which it is kneaded at a moderate temperature, for example at a temperature of 45° to 60°C, and then extruded through specially designed bores in an extruder head, which may be heated to the predetermined extrusion temperature, for example to around 45 to 50°C. The resulting strands are then pelletized.
- the temperature of the "molding compound" in the kneader is said to be an important parameter. Those molding compounds which are temperature sensitive may have to be cooled during the process to prevent destruction.
- the temperature of the mass immediately prior to its extrusion is at least 60°C; more preferably at least 70°C; most preferably at least 80°C.
- the temperature of the material may increase a few degrees as it is forced through the extrusion head.
- a specially designed extrusion head as there is with the method of US-A-5290496.
- any ordinary multi-aperture axial or radial extrusion head may be used.
- the apertures thereof may comprise plain cylindrical apertures of diameter not exceeding 2 mm; 0.5- 1.5 mm is a preferred range.
- Such apertures may be entirely cylindrical or may have a funnel portion on their upstream side, tapering to the main, cylindrical portion.
- the maximum temperature of the mass during the method should be such that there is no significant degradation.
- preferred sulphate and sulphonate anionic surfactants may be taken to temperatures well in excess of 80°C, without significant degradation; and in some cases up to 130°C.
- the maximum temperature of the material at any stage of the method does not exceed 100°C.
- the mass within the extruder is in a plastic and/or semi-solid form at least when it reaches the extrusion head.
- the mass is plastic and/or semi-solid when it is mechanically worked within the extruder.
- the mass is at an elevated temperature when mechanically worked, suitably at least 40°C; preferably at least 60°C; more preferably at least 70°C; most preferably at least 80°C.
- the feed material is added to the extruder at a temperature of at least 40°C, more preferably at least 60°C. It may be added as a solid or in plastic or molten form.
- the feed material is preferably an anionic surfactant paste, whose activity (i.e. anionic surfactant content) is suitably at least 40%wt, preferably at least 70%wt, most preferably at least 90%wt.
- the dried product is a waxy or pasty solid at ambient temperature, not a flowable powder.
- a feed material comprises an anionic surfactant which contains 2-10%wt of water, and whose activity is 90-98%wt. It is found that the presence of this water aids the processing of the surfactant, within the extruder and/or during a downstream spheronisation step, if carried out.
- a dried surfactant may be employed in the feed material, and there may be a separate addition of water to aid processing, either when the feed material is introduced to the extruder, or subsequently.
- the amount of water present after the addition may be as defined above. In preferred methods however no water is added to the extruder and the desired amount of water is preferably controlled by control of the water content of the feed material. This is preferably controlled not by adding water to a dried anionic surfactant, but by removing water to the extent required, in a prior surfactant drying process.
- the feed material is dried immediately prior to its introduction into the extruder.
- it is fed directly from a drier to the extruder, without being actively cooled therebetween.
- a non-ionic surfactant may aid the processing of the anionic surfactant within the extruder, and/or their downstream handling.
- an anionic surfactant and a non-ionic surfactant are present.
- the weight ratio of non-ionic surfactant to the anionic surfactant is suitably up to 1 part, preferably up to 0.5 parts, of non-ionic surfactant per part of anionic surfactant (with reference to their active contents).
- the higher alkyl group of such anionic surfactants is of 8 to 24, especially 10 to 20 carbon atoms, preferably 12 to 18 carbon atoms, and the alkoxylate content of such anionic surfactants that are alkoxylated (preferably ethoxylated or ethoxylated/propoxylated) is in the range of 1 to 4 alkoxy groups per mole.
- a preferred non-ionic surfactant is a condensation product of a higher fatty alcohol with a lower alkylene oxide, such as ethylene oxide or a mixture of ethylene oxide and propylene oxide.
- a lower alkylene oxide such as ethylene oxide or a mixture of ethylene oxide and propylene oxide.
- the higher fatty moiety will normally be of 12 to 15 carbon atoms and there will usually be present from 3 to 20, preferably 4 to 15 moles of alkylene oxide per mole of higher fatty alcohol.
- the particles contain a builder.
- a builder in particulate form is suitably added to the material comprising the anionic surfactant during or, preferably, prior to the mechanical working thereof.
- the builder is preferably not present during the drying step. It is preferably introduced subsequently, for example added to the material comprising the anionic surfactant prior to feeding into the extruder; at the time that material is fed into the extruder; or, preferably, subsequent to the feeding of the material comprising the anionic surfactant into the extruder, through a separate feed point.
- the builder when present, is added to the material comprising the anionic surfactant within the extruder during or, preferably, prior to the mechanical working thereof, said material already being at an elevated temperature, preferably at least 40°C, more preferably at least 60°C.
- Suitable builders include water soluble inorganic salt builders, preferably sodium salts, such as sodium polyphosphates, e.g. sodium tripolyphosphate and sodium pyrophosphate, sodium carbonate, sodium bicarbonate, sodium sesquicarbonate , sodium silicate, sodium disilicate, sodium metasilicate and sodium borate.
- water insoluble builders may also be useful, including the ion exchanging zeolites, such as Zeolite 4A.
- Organic builders may be employed but if heat sensitive may need to be added after extrusion.
- suitable organic builders are polyacetal carboxylates, as described in US-B-4725455, and water soluble salts of lower hydroxycarboxylic acids, such as sodium citrate and sodium gluconate.
- a builder when present, may suitably be present in an amount of from 0.1-10 parts per part of the anionic surfactant (active content), by weight.
- the anionic surfactant is, or is predominantly, an alkali metal alkyl sulphate
- the builder may suitably be present in an amount of from 0.2-6 parts per part of the anionic surfactant (active content), by weight, preferably 0.5-5, most preferably 0.7-4 parts, by weight.
- the builder may suitably be present in an amount of from 0.1-5 parts per part of the anionic surfactant (active content), by weight, preferably 0.1-1, most preferably 0.15-0.5 parts, by weight.
- a component for example a builder
- proportions of constituents are given herein there refer to the total content of the respective components , for example the total content of builders.
- the main ingredients of the extruded particles are preferably anionic surfactant and builder.
- Other constituents discussed already are water and non-ionic surfactant.
- adjuvants may be desirable for eventual detergent formulations. These may include a polymer, bleaching agent, optical brightener, sequestrant, conditioning agent, anti-foaming agent, filler, colorant, soil release agent, enzyme etc.
- a hydrotrope may be a useful adjuvant, firstly in preventing the anionic surfactant from becoming sticky as a result of water content and/or water absorption, and secondly in aiding washing processes, by promoting good dissolution. Examples of suitable hydrotropes are alkali metal arylsulphonates, for example sodium xylene sulphonate and sodium toluene sulphonate.
- adjuvants can be added to the material comprising the anionic surfactant prior to extrusion; for example prior to a prior drying step (when carried out); or subsequent to a prior drying step (when carried out) but prior to feeding of the material comprising the anionic surfactant into the extruder; or at the same time as that material is fed into the extruder; or subsequent to the feeding of the material comprising the anionic surfactant into the extruder, through one or more separate feed points, for example during or, preferably, prior to the mechanism working.
- adjuvants may be blended with the particles after their extrusion and cooling.
- adjuvants which are heat sensitive, such as enzymes post-extrusion blending may be preferred.
- the method of the present invention may produce particles which constitute a ready-to-use multi-component detergent or an intermediate product to be admixed or incorporated with other components, to produce a product for sale.
- an anionic surfactant in the form of a solid, semi-solid or paste is preferably fed in. It may be fed in in whatever way is most convenient - for example in lumps or shavings, or poured or pumped in. Other components may be co-fed, without a requirement for them to be carefully blended in; or may be added downstream, via one or more separate feed points.
- the mixing required to produce a good distribution of the components takes place within the extruder at an elevated temperature; and the mixing takes place most efficiently at temperatures which have previously been considered too high for the processing of the preferred sulphate and sulphonate anionic surfactants.
- the material in the extruder is plastic and/or semi-solid, and highly workable, at the temperature employed.
- the temperature of the material as it is extruded is higher than the melting or softening point of the anionic surfactant.
- the method may produce a granule containing a builder and an anionic surfactant, the primary elements of a detergent formulation, in one straightforward step from the as-supplied builder and surfactant; or in two steps if a prior drying step is employed, for drying the surfactant. No prior agglomeration step is required; indeed no prior mixing step of any kind is required, although prior mixing of certain adjuvants may be carried out, if this is the favoured way of incorporating them.
- an anionic surfactant, and a builder and other components when present, form an extrudate which has very good physical characteristics, even at temperatures at which the surfactant would normally be in a liquid state, and/or expected to hydrolyse or otherwise degrade.
- This allows intensive mixing within the extruder barrel, without the need for significant cooling of the mass prior to extrusion.
- compositions may be treated as a "dried” (solid) surfactant ingredient, without a downstream drying process; in preferred processes no forced or active drying process is carried out downstream of the extruder.
- the particles produced by the present invention are particularly suitable for use by formulators of laundry powders to deliver multiple ingredients into products .
- the particles may be admixed into a particulate blend of other ingredients, or may be partly ground, and re- agglomerated to give a fully formulated product.
- the prior art practice is to simply admix particles of relatively pure surfactant, particularly alkyl sulphates, into a powder.
- the invention offers the same ease of incorporation, with the benefits arising from the prior intimate mixing of the alkyl sulphate with other, often more readily soluble components. In the latter case, ease of formulation is improved by the delivery of multiple components, in the correct formulation ratio, suitably obtained by the process of the invention via a single solids addition.
- the invention offers a form of product which would be difficult for formulators to achieve without special equipment to make a densified powder.
- the process used is also more efficient than many formulators' own drying and blending operations, offering energy savings and reduced inventory.
- APV MP 2050 (trade mark) twin screw mixer-extruder was used, with 50 mm diameter screws, and a L:D ratio of 30:1.
- the barrel of the extruder was electrically heated and water cooled, with independently controlled heating zones. Unless otherwise stated the temperature was measured by means of thermocouples set into the inside surface of the barrel, at intervals along it.
- the extrusion was either axial extrusion through a standard 0.9 mm noodle plate or radial extrusion via a radial extrusion head, using a 1 mm mesh.
- the radial extrusion head allowed greater throughputs, and lower operating pressures. In general, for axial extrusions the operating pressures were relatively low, about 10 bar unless otherwise stated. For radial extrusions very low pressures were used; essentially no significant over pressure was applied.
- the anionic surfactant feeds were metered into the extruder using a weight-belt feeder. Builders and other solid ingredients were added using a screw feeder, with a loss in weight system. The builders were added at a distance of 9D from the surfactant feed. This allowed the surfactant feeds to be heated and worked, to become fully plastic, before builders were added.
- Extrudate temperature itself was measured by quickly collecting a mass of extrudate and immediately measuring the temperature in the centre of the mass by means of a thermocouple probe. Liquid additions were made using a volumetric pump.
- the particles were chopped into pieces in standard manner and then spheronisation was carried out in each case, using a CALEVA (trade mark) model 15 Disc spheroniser to give roughly spherical particles of approximately 1 mm diameter.
- CALEVA trade mark
- the surfactant used was a paste of sodium alkyl sulphate, based on a C 16.18 alcohol, containing about 70% surfactant (the remainder being water, sodium hydroxide, sodium sulphate, and unreacted alcohol), known as MANRO SNO (trade mark).
- MANRO SNO trade mark
- the molten as-prepared paste was allowed to cool until it solidified, and was broken into small pieces, to allow it to be fed into the extruder.
- the surfactant portion of the formulation was added as a molten liquid at about 80°C. It was observed that the temperature profile along the extruder barrel reflected the initial high temperature of the molten feed but from the mixing zone on, there was no significant difference between molten feed and solid feed. It was also demonstrated that using this form of feed material the extrudate could be produced at a rate of 80 kg/hr.
- the surfactant feed was based on sodium alkylbenzene sulphonate (LAS).
- the feed was made by drying a paste of 60% active LAS in a BALESTRA DRYEX (trade mark) wiped film evaporator, to an active content of 96-98%.
- the dried LAS was fed straight into the main feed port of the extruder at a temperature of 60°C, at a rate of 36.5 kg/hr.
- the surfactant was heated to 80°C and conveyed and to the mixing zone.
- the builder used was a blend of zeolite (VEGOBOND AX - trade mark) and sodium carbonate, in the ratio 3:1 wt:wt.
- the addition rate of builder was 27 kg/hr.
- the product was axially extruded through the 0.9 mm noodle die, at a higher pressure of 30 bar in this example, with an extrudate temperature of 90- 100°C.
- Sodium C 12 . 18 alkyl sulphate paste was previously dried, as described in the example above.
- the surfactant was fed into the extruder at a rate of 37.1 kg/hr. This was conveyed and heated to about 80°C.
- the builder was then added at a rate of 30.8 kg/hr.
- the builder was sodium disilicate and sodium carbonate, 3:1 wt:wt. It was observed that a small water addition (2.1 kg/hr) improved the downstream spheroniser performance.
- the extrusion was carried out using the radial extrusion head, with an extrusion temperature of 101°C.
- the product obtained contained 53% (w/w) of surfactant, 4% water and had a bulk density of 730 g/1.
- This product also gave a significant improvement in spheroniser performance, the product being more evenly sized with less dusting and reduced the extrusion temperature to 88°C, due to lesser heat gain during the passage through the extrusion head.
- This product contained 54% of anionic surfactant, 5% of non-ionic surfactant, and had a bulk density of 750 g/1.
- the dried sodium alkyl sulphate was fed at a rate of 18.2 kg/hr. This was conveyed and heated as previously.
- the builder (VEGOBOND AX zeolite only) was added at a rate of 29.3 kg/hr, and non-ionic surfactant was added at a rate of 2.5 kg/hr.
- the extrusion was via the axial head, at a temperature of 84°C.
- the product obtained contained 37% anionic surfactant, 5.2% non-ionic surfactant, and had a bulk density of 640 g/1.
- Dried sodium alkyl sulphate was fed as previously, at a rate of 10.7 kg/hr.
- Builder VEGOBOND AX zeolite : sodium carbonate, 11:1 wt:wt
- non-ionic surfactant was added at a rate of 4 kg/hr
- an acrylic-maleic polymer SOKOLAN CP5 (trade mark - an ingredient useful in laundry formulations) was added at a rate of 2.7 kg/hr.
- the temperature of the extrudate from the radial extruder was 80°C.
- the composition spheronised well.
- the product contained 20.2% anionic surfactant, 7.6% non-ionic surfactant, 5% polymer, and had a bulk density of 720 g/1.
- Sodium C 12 . 16 alkyl sulphate paste was dried as described in example 2.
- the surfactant was fed into the extruder at a rate of 50.0 kg/hr. This was conveyed and heated to 80°C. No builder or other components were added.
- the extrusion was carried out using the axial extrusion head with an extrusion temperature of 101°C.
- the product obtained was substantially pure surfactant particles of very high activity, and of bulk density of 600-750 g/1. The resultant particles could be handled and spheronised without difficulty.
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Abstract
Procédé de production de particules pour détergent à lessive. Le procédé est un procédé d'extrusion dans lequel un adjuvant pour détergent et un tensioactif, ce dernier contenant en tant que constituant principal un tensioactif anionique sulfaté ou sulfoné, sont envoyés dans une extrudeuse, travaillés mécaniquement à une température au moins égale à 40 °C puis extrudés par une tête d'extrudeuse comportant une multitude d'orifices d'extrusion. Le procédé d'extrusion permet de produire des particules de détergent ayant une masse volumique apparente qui est au moins égale à 400g/l et qui est de préférence comprise entre 550 et 900 g/l.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9726824.7 | 1997-12-19 | ||
GBGB9726824.7A GB9726824D0 (en) | 1997-12-19 | 1997-12-19 | Method of manufacturing particles |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1999032599A1 true WO1999032599A1 (fr) | 1999-07-01 |
Family
ID=10823870
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/GB1998/003791 WO1999032599A1 (fr) | 1997-12-19 | 1998-12-17 | Procede de production de particules |
Country Status (2)
Country | Link |
---|---|
GB (1) | GB9726824D0 (fr) |
WO (1) | WO1999032599A1 (fr) |
Cited By (28)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001085893A1 (fr) * | 2000-05-05 | 2001-11-15 | The Procter & Gamble Company | Procede de production de constituants nettoyants solides |
WO2002102959A1 (fr) * | 2001-06-19 | 2002-12-27 | Henkel Kommanditgesellschaft Auf Aktien | Produit de lavage et/ou produit de nettoyage pauvre en zeolithe et stable au stockage |
WO2004027009A1 (fr) * | 2002-09-12 | 2004-04-01 | Henkel Kommanditgesellschaft Auf Aktien | Produits de lavage ou de nettoyage comprimes sous l'effet d'une pression |
WO2010014395A1 (fr) * | 2008-07-28 | 2010-02-04 | The Procter & Gamble Company | Procédé pour la préparation d’une composition détergente |
EP2243822A1 (fr) | 2009-04-24 | 2010-10-27 | Unilever PLC | Poudre détergente dotée de particules riches en détergent |
WO2010122051A1 (fr) | 2009-04-24 | 2010-10-28 | Unilever Plc | Particules de détergent hautement actives |
WO2010122050A2 (fr) | 2009-04-24 | 2010-10-28 | Unilever Plc | Fabrication de particules détergentes extrêmement actives |
EP2441820A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Particules de détergent pour le lavage du linge |
EP2441821A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Particules de détergent pour le lavage du linge |
EP2441825A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Procédé pour la préparation de particules de détergent pour le lavage du linge |
EP2441822A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Particules de détergent pour le lavage du linge |
WO2012048947A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012048949A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particule de détergent à lessive |
WO2012048950A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012048948A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012049178A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent pour lessive |
WO2012049033A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Procédé à cuve à laver le linge à chargement par le haut |
WO2012048951A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2013149755A1 (fr) | 2012-04-03 | 2013-10-10 | Unilever Plc | Particules de détergent à lessive |
WO2013149753A1 (fr) | 2012-04-03 | 2013-10-10 | Unilever Plc | Particules de détergent à lessive |
WO2013149754A1 (fr) | 2012-04-03 | 2013-10-10 | Unilever Plc | Particules de détergent à lessive |
WO2013149752A1 (fr) | 2012-04-03 | 2013-10-10 | Unilever Plc | Particules de détergent à lessive |
US8883702B2 (en) | 2010-10-14 | 2014-11-11 | Conopco, Inc. | Packaged particulate detergent composition |
US9062281B2 (en) | 2010-10-14 | 2015-06-23 | Conopco, Inc. | Particulate detergent compositions comprising fluorescer |
US9365811B2 (en) | 2010-10-14 | 2016-06-14 | Conopco Inc. | Manufacture of coated particulate detergents |
KR20180034509A (ko) * | 2015-07-29 | 2018-04-04 | 제로스 리미티드 | 세척 방법, 장치 및 용도 |
IT201900003951A1 (it) * | 2019-03-19 | 2020-09-19 | Desmet Ballestra S P A | Impianto per la realizzazione di un prodotto, in particolare costituito da un prodotto tensioattivo |
CN111893008A (zh) * | 2020-08-10 | 2020-11-06 | 纳爱斯集团有限公司 | 一种洗涤制剂及其制备方法 |
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EP0328880A1 (fr) * | 1988-01-19 | 1989-08-23 | Colgate-Palmolive Company | Produit d'extrusion d'une composition détergente organique synthétique renforcée en forme particulaire et en forme de "petit pâté", et procédés de préparation et d'utilisation de ce dernier |
WO1991002047A1 (fr) * | 1989-08-09 | 1991-02-21 | Henkel Kommanditgesellschaft Auf Aktien | Fabrication de granules comprimes pour produits de lavage |
EP0508543A1 (fr) * | 1991-04-12 | 1992-10-14 | The Procter & Gamble Company | Structuration chimique de pâtes tensio-actives pour former des granulés tensio-actifs avec haute activité |
EP0663439A1 (fr) * | 1994-01-17 | 1995-07-19 | The Procter & Gamble Company | Procédé pour la préparation de granules de détergent |
JPH0827495A (ja) * | 1994-07-18 | 1996-01-30 | Lion Corp | 界面活性剤組成物の製造方法 |
DE19509752A1 (de) * | 1995-03-17 | 1996-09-19 | Henkel Kgaa | Verfahren zur Herstellung eines pulverförmigen Waschmittels |
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- 1997-12-19 GB GBGB9726824.7A patent/GB9726824D0/en not_active Ceased
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1998
- 1998-12-17 WO PCT/GB1998/003791 patent/WO1999032599A1/fr active Application Filing
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EP0328880A1 (fr) * | 1988-01-19 | 1989-08-23 | Colgate-Palmolive Company | Produit d'extrusion d'une composition détergente organique synthétique renforcée en forme particulaire et en forme de "petit pâté", et procédés de préparation et d'utilisation de ce dernier |
WO1991002047A1 (fr) * | 1989-08-09 | 1991-02-21 | Henkel Kommanditgesellschaft Auf Aktien | Fabrication de granules comprimes pour produits de lavage |
EP0508543A1 (fr) * | 1991-04-12 | 1992-10-14 | The Procter & Gamble Company | Structuration chimique de pâtes tensio-actives pour former des granulés tensio-actifs avec haute activité |
EP0663439A1 (fr) * | 1994-01-17 | 1995-07-19 | The Procter & Gamble Company | Procédé pour la préparation de granules de détergent |
JPH0827495A (ja) * | 1994-07-18 | 1996-01-30 | Lion Corp | 界面活性剤組成物の製造方法 |
DE19509752A1 (de) * | 1995-03-17 | 1996-09-19 | Henkel Kgaa | Verfahren zur Herstellung eines pulverförmigen Waschmittels |
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DATABASE WPI Section Ch Week 9614, Derwent World Patents Index; Class D25, AN 96-136605, XP002099513 * |
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WO2001085893A1 (fr) * | 2000-05-05 | 2001-11-15 | The Procter & Gamble Company | Procede de production de constituants nettoyants solides |
WO2002102959A1 (fr) * | 2001-06-19 | 2002-12-27 | Henkel Kommanditgesellschaft Auf Aktien | Produit de lavage et/ou produit de nettoyage pauvre en zeolithe et stable au stockage |
WO2004027009A1 (fr) * | 2002-09-12 | 2004-04-01 | Henkel Kommanditgesellschaft Auf Aktien | Produits de lavage ou de nettoyage comprimes sous l'effet d'une pression |
US8058222B2 (en) | 2008-07-28 | 2011-11-15 | The Procter & Gamble Company | Process for manufacturing extruded alkyl sulfate particles |
WO2010014395A1 (fr) * | 2008-07-28 | 2010-02-04 | The Procter & Gamble Company | Procédé pour la préparation d’une composition détergente |
EP2154235A1 (fr) | 2008-07-28 | 2010-02-17 | The Procter and Gamble Company | Procédé pour préparer une composition détergente |
EP2243822A1 (fr) | 2009-04-24 | 2010-10-27 | Unilever PLC | Poudre détergente dotée de particules riches en détergent |
WO2010122050A2 (fr) | 2009-04-24 | 2010-10-28 | Unilever Plc | Fabrication de particules détergentes extrêmement actives |
WO2010122050A3 (fr) * | 2009-04-24 | 2010-12-16 | Unilever Plc | Fabrication de particules détergentes extrêmement actives |
WO2010122051A1 (fr) | 2009-04-24 | 2010-10-28 | Unilever Plc | Particules de détergent hautement actives |
CN102414305A (zh) * | 2009-04-24 | 2012-04-11 | 荷兰联合利华有限公司 | 高活性洗涤剂颗粒的制备 |
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US9228157B2 (en) | 2009-04-24 | 2016-01-05 | Conopco, Inc. | Manufacture of high active detergent particles |
CN102414305B (zh) * | 2009-04-24 | 2014-07-23 | 荷兰联合利华有限公司 | 高活性洗涤剂颗粒的制备 |
US9284517B2 (en) | 2010-10-14 | 2016-03-15 | Conopco Inc. | Laundry detergent particle |
WO2012048947A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012048949A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particule de détergent à lessive |
WO2012048950A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012048948A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
WO2012049178A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent pour lessive |
WO2012049033A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Procédé à cuve à laver le linge à chargement par le haut |
WO2012048951A1 (fr) | 2010-10-14 | 2012-04-19 | Unilever Plc | Particules de détergent à lessive |
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EP2441825A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Procédé pour la préparation de particules de détergent pour le lavage du linge |
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EP2441821A1 (fr) | 2010-10-14 | 2012-04-18 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Particules de détergent pour le lavage du linge |
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US11414633B2 (en) * | 2015-07-29 | 2022-08-16 | Xeros Limited | Cleaning method, apparatus and use |
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IT201900003951A1 (it) * | 2019-03-19 | 2020-09-19 | Desmet Ballestra S P A | Impianto per la realizzazione di un prodotto, in particolare costituito da un prodotto tensioattivo |
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Also Published As
Publication number | Publication date |
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GB9726824D0 (en) | 1998-02-18 |
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