AU2002358221A1 - Improvements relating to smokable filler materials - Google Patents
Improvements relating to smokable filler materials Download PDFInfo
- Publication number
- AU2002358221A1 AU2002358221A1 AU2002358221A AU2002358221A AU2002358221A1 AU 2002358221 A1 AU2002358221 A1 AU 2002358221A1 AU 2002358221 A AU2002358221 A AU 2002358221A AU 2002358221 A AU2002358221 A AU 2002358221A AU 2002358221 A1 AU2002358221 A1 AU 2002358221A1
- Authority
- AU
- Australia
- Prior art keywords
- filler material
- agglomerated
- tobacco filler
- tobacco
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 165
- 239000000945 filler Substances 0.000 title claims abstract description 128
- 241000208125 Nicotiana Species 0.000 claims abstract description 210
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 210
- 239000011230 binding agent Substances 0.000 claims abstract description 61
- 239000000428 dust Substances 0.000 claims abstract description 46
- 230000000391 smoking effect Effects 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims description 19
- 239000008187 granular material Substances 0.000 claims description 11
- 238000003801 milling Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003906 humectant Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 235000010987 pectin Nutrition 0.000 claims description 8
- 239000001814 pectin Substances 0.000 claims description 8
- 229920001277 pectin Polymers 0.000 claims description 8
- 239000005913 Maltodextrin Substances 0.000 claims description 7
- 229920002774 Maltodextrin Polymers 0.000 claims description 7
- 229940035034 maltodextrin Drugs 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 235000010443 alginic acid Nutrition 0.000 claims description 6
- 229920000615 alginic acid Polymers 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims description 6
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 5
- 229940072056 alginate Drugs 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
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000008119 colloidal silica Substances 0.000 claims description 2
- 239000000796 flavoring agent Substances 0.000 claims description 2
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 239000010451 perlite Substances 0.000 claims description 2
- 235000019362 perlite Nutrition 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000010455 vermiculite Substances 0.000 claims description 2
- 229910052902 vermiculite Inorganic materials 0.000 claims description 2
- 235000019354 vermiculite Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 235000019505 tobacco product Nutrition 0.000 description 9
- 238000005054 agglomeration Methods 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000010407 ammonium alginate Nutrition 0.000 description 2
- 239000000728 ammonium alginate Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 230000008570 general process Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 244000215068 Acacia senegal Species 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 229920000936 Agarose Polymers 0.000 description 1
- 244000106483 Anogeissus latifolia Species 0.000 description 1
- 235000011514 Anogeissus latifolia Nutrition 0.000 description 1
- 241000416162 Astragalus gummifer Species 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 240000008886 Ceratonia siliqua Species 0.000 description 1
- 235000013912 Ceratonia siliqua Nutrition 0.000 description 1
- 244000303965 Cyamopsis psoralioides Species 0.000 description 1
- 235000017788 Cydonia oblonga Nutrition 0.000 description 1
- 229920000855 Fucoidan Polymers 0.000 description 1
- SNVFDPHQAOXWJZ-UHFFFAOYSA-N Furcelleran Chemical compound CCOC(=O)C1=C(C)NC(C=2C=CC=CC=2)=C(C(=O)OCC=2C=CC=CC=2)C1C#CC1=CC=CC=C1 SNVFDPHQAOXWJZ-UHFFFAOYSA-N 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- 239000001922 Gum ghatti Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- 240000007472 Leucaena leucocephala Species 0.000 description 1
- 241001364096 Pachycephalidae Species 0.000 description 1
- HDSBZMRLPLPFLQ-UHFFFAOYSA-N Propylene glycol alginate Chemical compound OC1C(O)C(OC)OC(C(O)=O)C1OC1C(O)C(O)C(C)C(C(=O)OCC(C)O)O1 HDSBZMRLPLPFLQ-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000015125 Sterculia urens Nutrition 0.000 description 1
- 240000001058 Sterculia urens Species 0.000 description 1
- 229920001615 Tragacanth Polymers 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- VEUACKUBDLVUAC-UHFFFAOYSA-N [Na].[Ca] Chemical compound [Na].[Ca] VEUACKUBDLVUAC-UHFFFAOYSA-N 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- KPGABFJTMYCRHJ-YZOKENDUSA-N ammonium alginate Chemical compound [NH4+].[NH4+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O KPGABFJTMYCRHJ-YZOKENDUSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 235000010410 calcium alginate Nutrition 0.000 description 1
- 239000000648 calcium alginate Substances 0.000 description 1
- 229960002681 calcium alginate Drugs 0.000 description 1
- DIOLOCSXUMYFJN-UHFFFAOYSA-N calcium;azane Chemical compound N.[Ca+2] DIOLOCSXUMYFJN-UHFFFAOYSA-N 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 229920001525 carrageenan Polymers 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 fibres Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000019314 gum ghatti Nutrition 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 238000010915 one-step procedure Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 235000010408 potassium alginate Nutrition 0.000 description 1
- 239000000737 potassium alginate Substances 0.000 description 1
- MZYRDLHIWXQJCQ-YZOKENDUSA-L potassium alginate Chemical compound [K+].[K+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O MZYRDLHIWXQJCQ-YZOKENDUSA-L 0.000 description 1
- 235000010409 propane-1,2-diol alginate Nutrition 0.000 description 1
- 239000000770 propane-1,2-diol alginate Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/12—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
- A24B15/14—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco made of tobacco and a binding agent not derived from tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24C—MACHINES FOR MAKING CIGARS OR CIGARETTES
- A24C5/00—Making cigarettes; Making tipping materials for, or attaching filters or mouthpieces to, cigars or cigarettes
- A24C5/01—Making cigarettes for simulated smoking devices
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Catching Or Destruction (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
The present invention provides an agglomerated tobacco filler material comprising dust and binder, the tobacco dust and binder being present at greater than 650 by weight of the agglomerated tobacco filler material, the material having a fill value substantially similar to the fill value of cut tobacco. The present invention further provides a method of making the agglomerated tobacco filler material of the present invention, and a smoking article incorporating said material.
Description
WO 03/055337 PCT/GB02/05899 1 Improvements relating to Smokable Filler Materials The subject invention relates to smokable filler materials and more particularly to agglomerated tobacco filler material, and smoking articles incorporating such material. As a result of primary and secondary processing, dust and fines of no further commercial use are produced. The fine tobacco may have a high silica content, which because of its abrasive nature renders the fine tobacco less than desirable for use in a further process which utilises cutting or grinding apparatus. The fine tobacco waste that cannot currently be processed further is taken for landfill. In the current economic climate reduction of landfill is desirable for financial and environmental reasons. Any process which maximises tobacco waste usage has great benefit. Paper-making processes currently used for making reconstituted tobacco products need a high throughput to make them efficient and cost effective. Paper-making processes may not be suitable for certain factories due to lack of expensive apparatus or low volume of materials. Any process utilising waste without the need for high cost apparatus would be of significant benefit.
WO 03/055337 PCT/GB02/05899 2 The utilisation of some tobacco dust in reconstituted products is long since known, for example in products such as reconstituted sheet material, bandcast sheet and extrusion products as previously described in our patents GB 2201081 and GB 2201080. Such products utilise processed tobacco dust and can be incorporated into smoking articles at inclusion levels of up to 30% by weight of material in the tobacco rod. Some of these products, in particular bandcast sheet and products of extrusion, have poor handling properties and are susceptible to degradation during further processing. Such reconstituted products have fill values in the range of 2.5cm 3 /g to 3.5cm3/g, these fill values being substantially lower than those of cut tobacco (5cm 3 /g to 6cm 3 /g) and reconstituted tobacco sheet (8.0cm 3 /g to 8.5cm 3 /g). The agglomeration of tobacco dust and fines has been previously proposed as a means of generating reconstituted tobacco products. In US 3,894,544 a process for the production of reconstituted tobacco material is described in which ribs and wastes are moistened with a liquid, kneaded together to form a dough-like mass which is then shaped to form leaf-like structures. The leaf-like structures are spread under pressure to form individual flakes.
WO 03/055337 PCT/GB02/05899 3 DE 3 312 159 describes a method of manufacture for tobacco leaf-like material by pelletising a mixture of fine tobacco particles, fibres, water and binder and rolling out the pellets to a desired thickness to give a material that may be added directly to cut tobacco. US 4,341,228 describes a process in which tobacco dust is mixed with a bonding material, the mixture is then treated so as to form agglomerated fibres. These agglomerated fibres are mixed with tobacco-parts in a slurry and formed into a sheet by means of a paper-making process. That sheet is then dried and shredded. The agglomerated tobacco dust particles are of a size such that they do not pass through a 56 mesh screen, and preferably do not pass through a 20 mesh (0.84mm) screen. Each of these methods results in a product through compaction with added binders thereby resulting in a dense reconstituted tobacco product. It is an object of the present invention to provide an agglomerated tobacco product in which tobacco waste, and in particular tobacco dust currently of no commercial value may be utilised to give a product having a fill value substantially similar to that of cut tobacco. It is a further object of the present invention to provide an agglomerated tobacco product which can use waste of high silica content, such waste usually being of no commercial value in conventional reconstituted tobacco WO 03/055337 PCT/GB02/05899 4 products and processes due to silica being highly abrasive to grinders and cutters used in further processing. It is an even further object of the present invention to provide an agglomerated tobacco product capable of being used instead of, or in combination with, other reconstituted tobacco material in smoking articles, wherein the fill value of the agglomerated tobacco filler material is substantially similar to that of cut tobacco. It is a yet further object of the present invention to provide an agglomerated tobacco filler material having acceptable handling properties and reduced frangibility such that the product may be directly incorporated into smoking articles without the need for further processing. The present invention also has as an object an agglomerated tobacco filler material that is produced using fluidised bed technology and low process temperatures in a one-step procedure. As referred to herein, 'fill value' shall be taken as meaning the volume measured in cubic centimetres taken up by 1 gram of product. Fill value is measured using a Borgwaldt Densimeter (DD 60A) by taking a known weight of sample contained in a stainless steel cylinder of known dimensions, for example a cylinder of 3cm radius, and subjecting the sample to pressure from a weighted piston (for example 1kg extra weight) for 30 seconds. The WO 03/055337 PCT/GB02/05899 5 residual height of the compressed sample is measured and converted to volume. Results are recorded in cm 3 /g. Measurements of fill value were done with the equipment described. Bulk density shall be taken as meaning the weight of product (grams) per unit volume (cm 3 ). Results are recorded in g/cm 3 . The present invention provides an agglomerated tobacco filler material comprising tobacco dust and binder, the amount of tobacco dust and binder being greater than 65% by weight of the agglomerated tobacco filler material, said agglomerated tobacco filler material having a fill value substantially similar to the fill value of cut tobacco. Preferably the tobacco dust and binder are present at more than about 70% by weight of the agglomerated tobacco filler material, more preferably the tobacco dust and binder are present at more than about 75% by weight, and even more preferably at more than about 80% by weight. Even more preferably the tobacco dust and binder are present at more than about 85% by weight and most preferably are present at more than about 90% by weight of the agglomerated tobacco filler material. Preferably the agglomerated tobacco filler material has a fill value in the range of about 4.40cm 3 /g to about WO 03/055337 PCT/GB02/05899 6 5.50cm 3 /g, and more preferably is in the range of about 4.90cm 3 /g to about 5.30cm?/g. Preferably the agglomerated tobacco filler material has a granule size up to about 3.5mm. More preferably the granule size is at least 0.7mm and not more than about 2.0mm. Most preferably the granule size is in the range of about 0.8mm to about 2.0mm. Preferably the agglomerated tobacco filler material has a moisture content in the range of about 8% to about 18%. More preferably the agglomerated tobacco filler material has a moisture content in the range of about 10% to about 15.5%. The agglomerated tobacco filler material of the present invention advantageously has a bulk density substantially similar to that of cut tobacco. The bulk density value of a product is essentially equal to the reciprocal of the fill value for that product. For the agglomerated tobacco filler material the bulk density should advantageously be matched to that of cut tobacco, such that the agglomerated tobacco filler material will have a reduced tendency to de-blend when compared with products, such as the products described in GB 2201081, having a bulk density substantially dissimilar to that of cut tobacco. Preferably the bulk density of the agglomerated tobacco filler material is in the range 0.10g/cm 3 to WO 03/055337 PCT/GB02/05899 7 0.33g/cm 3 , and more preferably is in the range 0.12g/cm 3 to 0.25g/cm 3 , and even more preferably is in the range 0.12g/cm 3 to 0.14g/cm 3 . Most preferably the bulk density of the agglomerated tobacco filler material is about 0.14g/cm. Advantageously, the agglomerated tobacco filler material comprises tobacco dust at more than about 70% by weight, preferably more than about 75% by weight. Even more preferably tobacco dust is present in the range of about 75% to about 95% by weight of the agglomerated material. The agglomerated tobacco filler material suitably comprises tobacco dust in the range of about 80% to about 90% by weight of the agglomerated material. The agglomerated tobacco filler material further comprises a binder, wherein the binder is preferably present in the range of about 1% to about 15% by weight of the agglomerated material. More preferably the binder is present in the range of about 1.5% to about 8% by weight, and is more preferably in the range of about 3.0% to about 6% by weight, and even more preferably is about 5% by weight of the agglomerated material. When the binder is maltodextrin, the binder is advantageously present in the range of about 1% to about 30% by weight of the agglomerated material. More preferably when the binder is maltodextrin the binder is present at about 27% by weight of the agglomerated material.
WO 03/055337 PCT/GB02/05899 8 Suitably the binder is selected from the group consisting of organic binders, such as an alginate, a gum, a cellulose (modified or natural), a pectin or pectinaceous binder, or the Group I or II metal salts of these binders, such as sodium carboxymethylcellulose (NaCMC), or sodium alginate; maltodextrin or polyvinylpyrrolidine (PVP). Much preferred binders are pectinaceous binders, and most preferably the binder is a pectin. Other organic binders include soluble alginates, such as ammonium alginate, sodium alginate, sodium calcium alginate, calcium ammonium alginate, potassium alginate, triethanolamine alginate and propylene glycol alginate. Cellulosic binders include, for example, cellulose derivatives, such as sodium carboxymethylcellulose, methylcellulose, hydroxylpropylcellulose (HPC), hydroxylethylcellulose or cellulose ethers. Other binders include gums such as gum arabic, gum ghatti, gum tragacanth, Karaya, locust bean, acacia, guar, quince seed or xanthan gum, or gels such as, agar, agarose, carrageenans, fucoidan and furcelleran. Starches can also be used as organic binders. Other suitable gums can be selected by reference to handbooks, such as 'Industrial Gums', Ed. Whistler (Academic Press).
WO 03/055337 PCT/GB02/05899 9 Other suitable binders will be known to a person skilled in the art. The agglomerated tobacco filler material may additionally comprise a humectant. The humectant may suitably be one or-more of glycerol, sorbitol, diethylene glycol and propylene glycol. Other suitable humectants will be known to a person skilled in the art. Preferably the humectant is present in the range of 1% to about 5% by weight of the agglomerated material. The humectant improves the flexibility and the moisture content of the agglomerated tobacco filler material such that the filler material is more robust during handling and storage. The agglomerated tobacco filler material may additionally comprise inert fillers and/or flavourant material. Suitably the inert filler may be one or more of the group consisting of silicates or alumino-silicates, such as perlite, vermiculite, diatomaceous earth, talc or colloidal silica; chalk, or metal oxides, metal salts or hydroxides such as magnesium oxide, magnesium sulphate, calcium or magnesium carbonate or alumina, or other inert fillers known to those skilled in the art. The present invention also provides a smoking article comprising a rod of smokable material wrapped in a wrapper, wherein agglomerated tobacco filler material WO 03/055337 PCT/GB02/05899 10 of the present invention is blended with cut tobacco and/or reconstituted tobacco. Preferably the agglomerated tobacco filler material is present at up to about 25% by weight of the smokable material of the smoking article and more preferably is present at up to about 20% by weight of the smokable material. More preferably the agglomerated tobacco filler material is present in the range of about 2% to aboutl0% by weight of the smokable material, and is even more preferably present in the range of about 5% to about 6% by weight of the smokable material. The agglomerated tobacco filler material used in a smoking article of the present invention advantageously has a granule size in the range of about 0.7mm to about 3.5mm, preferably in the range of about 0.8mm to about 1.4mm and/or a granule size in the range of about 1.4mm to about 2.0mm. Agglomerated tobacco filler material having a granule size of less than 0.5mm may suitably be used in subsequent agglomeration steps. Agglomerated tobacco filler material having a granule size greater than 3.5mm may be ground to a suitable particle size and reused in subsequent agglomeration steps. Preferably a smoking article incorporating the agglomerated tobacco filler material of the present WO 03/055337 PCT/GB02/05899 11 invention has a static burn rate substantially similar to a smoking article incorporating blended Virginia tobacco having 10% reconstituted tobacco sheet. Advantageously a smoking article incorporating the agglomerated tobacco filler material of the present invention has a firmness value substantially similar to that of a smoking article incorporating a standard Virginia blend having 10% reconstituted tobacco sheet. The present invention further provides a robust agglomerated tobacco filler material having improved handling properties. This is particularly advantageous in view of degradation suffered in tobacco primary and secondary processing stages. The agglomerated tobacco filler material has a robustness measured in accordance with the method described in Example 3 below. Robustness may be expressed as the loss of agglomerated tobacco filler material during the milling process, i.e. it is a measure of the size reduction of granules as a result of degradation. Loss of agglomerated product is the difference between the percentage of agglomerated tobacco filler material retained on sieves of greater then 710pm before milling and the percentage of agglomerated tobacco filler material retained on sieves of greater then 710Rm after milling.
WO 03/055337 PCT/GB02/05899 12 Preferably the loss after milling is less than about 45% by weight of agglomerated tobacco filler material, more preferably the loss after milling is less than about 40% by weight of agglomerated material. The loss after milling is even more preferably less than about 32% by weight and is most preferably less than about 20% by weight of agglomerated tobacco filler material. The robustness of the agglomerated product may depend upon the binder used in the agglomeration process. The effectiveness of the binders in making a robust product may be listed from most effective to least effective as Apple Pectin > PVP > HPC > Alginate > Maltodextrin > CMC. Preferably the binder providing the most robust agglomerated tobacco filler material is Apple pectin. The present invention further provides a method of producing the agglomerated tobacco filler material of the present invention, wherein tobacco dust of particle size not more than 500pm is fluidised in a stream of warm air and binder is applied to said fluidised tobacco dust, such that an agglomerated tobacco filler material is produced having a fill value substantially similar to that of cut tobacco. Preferably the inlet temperature of the air is not more than 80 0 C. Suitably the binder is sprayed onto the fluidised tobacco dust at a spray rate in the range of about WO 03/055337 PCT/GB02/05899 13 0.01431/min/kg tobacco dust to about 0.0571/min/kg tobacco dust. Preferably the spray rate is about 0.02861/min/kg tobacco dust. Suitably the tobacco dust and binder are mixed using the method of the present invention for between 20 and 60 minutes. Preferably the agglomerated tobacco filler material produced by the method of the present invention has a fill value substantially similar to that of cut tobacco. In order that the invention may be easily understood and readily carried into effect, reference will now be made to the following examples. Example 1 Tobacco dust is ground to give a particle size of less than 500Am diameter and a bulk density of between 0.3g/cm 3 and 0.38g/cm 3 . 300-350g of tobacco dust is loaded into the product container of an Aeromatic-Fielder STREA-1. The instrument is operated using the top spray nozzle and an inlet air temperature of 60 0 C. The outlet air temperature is in the range of 27 to 39 0 C. The dust is then fluidised in a stream of warm air. The agglomeration fluid, containing the binder, is sprayed onto the fluidised tobacco dust at a spray rate of WO 03/055337 PCT/GB02/05899 14 approximately 10ml/min. for between 20 and 60 minutes. The resulting agglomerated tobacco product is thus agglomerated and dried in a single operation. The moisture content of the agglomerated tobacco filler material at the end of the agglomeration process is between 12 and 16%, and is ideally about 14%. Before incorporation into a smoking article, the agglomerated tobacco filler material is conditioned to a moisture content of between 11% and 16%. Table 1 shows the fill values for three different tobacco blends and respective agglomerated tobacco filler materials made according to the general method described in Example 1 using Apple pectin as a binder (5% by weight of the agglomerated product). Table 1: Fill Values for Tobacco and Agglomerated Tobacco Sample Moisture (%) Fill Value (cc/g) Virginia Tobacco 13.5 5.44 Virginia Agglomerate 11.8 5.28 Burley Tobacco 13.5 5.40 Burley Agglomerate 13.9 4.47 USB Tobacco 13.5 5.29 USB Agglomerate 11.9 4.97 Example 2 Agglomerated tobacco filler material made according to the general process described in Example 1 comprising WO 03/055337 PCT/GB02/05899 15 tobacco dust at 92% by weight, 3% by weight humectant and 5% by weight binder. Example 3 The robustness of the agglomerated tobacco product was determined for agglomerates formed using a number of different binders. A Pascall Ball-Mill, having six balls each weighing 22.5g, was used at Speed 9 for a 30 second duration with 10 grams of agglomerated tobacco product. The percentage weight of agglomerated tobacco filler material retained on a sieve of particular screen size before and after milling was recorded, and the frangibility calculated for the different samples. Frangibility was calculated for each sieve of given screen size as: Frang (%) = Agglomerate after milling (%) - Agglomerate before milling (%) The results of the frangibility tests are shown in Table 2.
WO 03/055337 PCT/GB02/05899 16 Table 2: Results of Ball-Milling Tests and Frangibility of Agglomerates BINDER% MILLING 1400um 1000um 710um 500um 355um BASE MC% Apple pectin 5.6% Initial % 62.1 24.9 7.4 3.0 1.1 1.5 After mill % 22.6 36.2 18.8 10.9 4.7 6.8 Frang % -39.5 11.3 11.4 7.9 3.6 4.3 13.7 PVP 4% Initial % 0.2 6.4 33.1 36.6 14.0 9.7 After mill % 0.1 0.5 7.9 35.1 28.7 27.7 Frang % -0.1 -5.9 -25.2 -1.5 14.7 18.0 15.0 Maltodextrin 27% Initial % 1.4 13.5 32.7 30.5 13.3 8.6 After mill % 0.1 0.7 6.8 32.8 29.9 29.7 Frang % -1.3 -12.8 -25.9 2.3 16.6 21.1 13.1 HPC 1.7% Initial % 0.9 12.3 37.9 31.7 10.7 6.5 SAfter mill % 0.2 1.7 13.8 36.0 24.1 24.2 Frang % -0.7 -10.6 -24.1 4.3 13.4 17.7 16.9 CMC4.15% Initial % 34.9 35.6 15.6 7.4 2.8 3.7 After mill % 3.1 11.6 26.4 27.8 14.0 17.2 Frang % -31.8 -24.0 10.8 20.4 11.2 13.5 18.0 Alginate 6.7% Initial % 29.7 42.3 15.4 6.9 2.2 3.5 After mill % 1.1 16.1 31.3 27.4 11.3 12.8 Frang % -28.6 -26.2 15.9 20.5 9.1 9.3 14.6 Apple pectin 5.5% Initial % 76.3 17.3 3.7 1.1 0.3 1.3 After mill % 45.0 29.4 12.0 6.4 2.6 4.6 Frang % -31.3 12.1 8.3 5.3 2.3 3.3 15.2 Example 4 Using a STREA-1 fluidised bed and 350g of tobacco dust and a final binder concentration on the agglomerates of 5% weight/weight, a particle size distribution curve was produced for 6 agglomeration runs. The agglomerated particle size distribution is shown in Table 3.
WO 03/055337 PCT/GB02/05899 17 Table 3: Sieve Analysis of Tobacco Dust and Tobacco Agglomerates Size (microns) Agglomerate(%) Tobacco dust(%) Run 1 Run 2 Run 4 Run 5 Run 6 Starting Material 2000 - - 19 12 - 1400 38 44 49 35 15 1000 29 34 23 31 45 710 11 12 6 10 22 500 7 6 2 6 11 1 355 4 2 1 3 4 24 250 3 2 - 1 2 22 150 3 - - - - 27 Base 5 - - 2 1 26 Example 5 A tobacco blend comprising 6.3kg of blended tobacco minus the standard '10% Reconstituted Tobacco Sheet (RTS) component and 0.7kg (10% by weight) of agglomerated tobacco filler material of 800gm to 1400Im was produced thus using the agglomerated tobacco filler material as an alternative to reconstituted tobacco. Example 6 A tobacco blend comprising 6.3kg of blended tobacco minus the standard 10% RTS component and 0.7kg (10% by weight) of agglomerated tobacco filler material of 1400pm to 2000pm was produced thus using the agglomerated tobacco filler material as an alternative to reconstituted tobacco. Example 7 A tobacco blend comprising 6.65kg of blended tobacco inclusive of the standard 10% RTS component and WO 03/055337 PCT/GB02/05899 18 0.35kg (5% by weight) of agglomerated tobacco filler material of 8004m to 1400pm was produced thus using the agglomerated tobacco filler material in combination with reconstituted tobacco. Example 8 Agglomerated tobacco filler material was made according to the general process described in Example 1 further comprising inert filler material. The agglomerated tobacco filler material comprised 76% by weight tobacco dust, 19% by weight inert filler material and 5% by weight binder. Example 9 The static burn rates, firmness and ends stability results for smoking articles incorporating the agglomerated tobacco filler material of the present invention are listed in Table 4.
WO 03/055337 PCT/GB02/05899 19 a) 421 U3 .1-4 0 41I (d1 In Q)
H
U 4.) -H 41) 42 44 44 0 0 0 0- r- ('40'3 ,-4 -' (1) %D00' ca ( '00 aa) 00 a) -. t'H.4 -1 In U0 In 0 In 411 oE .14-) 4.)H H i 00 0 ~ II) u 0 Hd H) 0 7t) H i H al .o En Ea WO 03/055337 PCT/GB02/05899 20 Example 10 Physical measurements for smoking articles incorporating the agglomerated tobacco filler material of the present invention are listed in Table 5. It is interesting to note that as the fill value of the agglomerate is less than that of the tobacco blend, the density of a smoking article incorporating the agglomerated tobacco filler material would be expected to be higher than that of a smoking article not containing the agglomerated material. Instead the physical measurements show that the density of smoking articles incorporating the agglomerated product are lower than smoking articles not containing the agglomerated material.
WO 03/055337 PCT/GB02/05899 21 LO U) 4 P4- 0 1 r14 4) 0 H .L2 bll Vr4 0 I-I a) H r n ~ 4.a) 0 00 O) 0 0H 0 r40 41)$ 0 HH) N 0 a o~ H rd 0 ,cI, E- HH co 0MI C C 0) 00 4JU
Claims (43)
1. An agglomerated tobacco filler material comprising tobacco dust and binder, the amount of. tobacco dust and binder being greater than 65% by weight of the agglomerated tobacco filler material, said agglomerated tobacco filler material having a fill value substantially similar to the fill value of cut tobacco.
2. An agglomerated tobacco filler material according to Claim 1, wherein the tobacco .dust and binder are present at more than about 70% by weight of the agglomerated tobacco filler material.
3. An agglomerated tobacco filler material according to Claim 2, wherein the tobacco dust and binder are present at more than about 75% by weight.
4. An agglomerated tobacco filler material according to Claim 3, wherein the tobacco dust and binder are present at more than about 80% by weight.
5. An agglomerated tobacco filler material according to Claim 4, wherein the tobacco dust and binder are present at more than about 85% by weight.
6. An agglomerated tobacco filler material according to Claim 5, wherein the tobacco dust and binder are present at more than about 90% by weight. WO 03/055337 PCT/GB02/05899 23
7. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material has a fill value in the range of about 4.40cm 3 /g to about 5.50cm 3 /g.
8. An agglomerated tobacco filler material according to Claim 7, wherein said fill value is in the range of about 4.90cm 3 /g to about 5.30cm 3 /g.
9. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material has a granule size up to about 3.5mm.
10. An agglomerated tobacco filler material according to Claim 9, wherein said granule size is at least 0.7mm and not more than about 2.0mm.
11. An agglomerated tobacco filler material according to Claim 10, wherein said granule size is in the range of about 0.8mm to about 2.0mm.
12. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material has a moisture content in the range of about 8% to about 18%.
13. An agglomerated tobacco filler material according to Claim 12, wherein said moisture content is in the range of about 10% to about 15.5%.
14. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said WO 03/055337 PCT/GB02/05899 24 agglomerated tobacco filler material has a bulk density substantially similar to that of cut tobacco.
15. An agglomerated tobacco filler material according to Claim 14, wherein said bulk density is in the range 0.10g/cm' to 0.33g/cm 3 .
16. An agglomerated tobacco filler material according to Claim 15, wherein said bulk density is in the range 0.12g/cm 3 to 0.25g/cm.
17. An agglomerated tobacco filler material according to Claim 16, wherein said bulk density is in the range 0.12g/cm 3 to 0.14g/cm.
18. An agglomerated tobacco filler material according to Claim 17, wherein said bulk density is about 0.14g/cm 3 .
19. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material comprises tobacco dust at more than about 70% by weight.
20. An agglomerated tobacco filler material according to Claim 19, wherein said agglomerated tobacco filler material comprises tobacco dust at more than about 75% by weight.
21. An agglomerated tobacco filler material according to Claim 20, wherein said tobacco dust is present in the range of about 75% to about 95% by weight of the agglomerated material. WO 03/055337 PCT/GB02/05899 25
22. An agglomerated tobacco filler material according to Claim 21, wherein said tobacco dust is present in the range of about 80% to about 90% by weight of the agglomerated material.
23. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said binder is preferably present in the range of about 1% to about 15% by weight of the agglomerated material.
24. An agglomerated tobacco filler material according to Claim 23, wherein said binder is present in the range of about 1.5% to about 8% by weight.
25. An agglomerated tobacco filler material according to Claim 24, wherein said binder is present in the range of about 3.0% to about 6% by weight.
26. An agglomerated tobacco filler material according to Claim 25, wherein said binder is about 5% by weight of the agglomerated material.
27. An agglomerated tobacco filler material according to any one of the Claims 1-22, wherein when the binder is maltodextrin, said binder is present in the range of about 1% to about 30% by weight of the agglomerated material.
28. An agglomerated tobacco filler material according to Claim 27, wherein when the binder is maltodextrin said binder is present at about 27% by weight of the agglomerated material. WO 03/055337 PCT/GB02/05899 26
29. An agglomerated tobacco filler material according to any one of claims 1-26, wherein the binder is selected from the group consisting of organic binders, such as an alginate, a gum, a cellulose (modified or natural), a pectin or pectinaceous binder, or the Group I or II metal salts of these binders, such as sodium carboxymethylcellulose (NaCMC), or sodium alginate; or polyvinylpyrrolidine (PVP).
30. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material comprises a humectant.
31. An agglomerated tobacco filler material according to Claim 30, wherein said humectant is one or more of glycerol, sorbitol, diethylene glycol and propylene glycol.
32. An agglomerated tobacco filler material according to Claim 30 or 31, wherein said humectant is present in the range of 1% to about 5% by weight of. the agglomerated material.
33. An agglomerated tobacco filler material according to any one of the preceding claims, wherein said agglomerated tobacco filler material comprises inert fillers and/or flavourant material. WO 03/055337 PCT/GB02/05899 27
34. An agglomerated tobacco filler material according to Claim 33, wherein said inert filler material is one or more of the group consisting of silicates or alumino-silicates, such as perlite, vermiculite, diatomaceous earth, talc or colloidal silica; chalk, or metal oxides, metal salts or hydroxides such as magnesium oxide, magnesium sulphate, calcium or magnesium carbonate or alumina.
35. An agglomerated tobacco filler material according to any one of Claims 1-34, wherein the loss after milling is less than about 45% by weight of the agglomerated tobacco filler material.
36. A smoking article comprising a rod of smokable material wrapped in a wrapper, wherein said smokable material comprises agglomerated tobacco filler material according to any one of Claims 1-35 blended with cut tobacco and/or reconstituted tobacco.
37. A smoking article according to Claim 36, wherein said agglomerated tobacco filler material is present at up to about 25% by weight of the smokable material.
38. A smoking article according to Claim 37, wherein said agglomerated tobacco filler material is present at up to about 20% by weight of smokable material.
39. A smoking article according to Claim 38, wherein said agglomerated tobacco filler material is present in WO 03/055337 PCT/GB02/05899 28 the range of about 2% to about 10% by weight of the smokable material.
40. A smoking article according to Claim 39, wherein said agglomerated tobacco filler material is present in the range of about 5% to about 6% by weight of the smokable material.
41. A method of producing the agglomerated tobacco filler material of any one of Claims 1-35, wherein tobacco dust of particle size not more than 500pm is fluidised in a stream of warm air and binder is applied to said fluidised tobacco dust, such that an agglomerated tobacco filler material is produced having a fill value substantially similar to that of cut tobacco.
42. An agglomerated tobacco filler material substantially as hereinabove described with reference to the Examples hereof.
43. A smoking article substantially as hereinabove described with reference to the Examples hereof.
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| GB0130627.3 | 2001-12-21 | ||
| PCT/GB2002/005899 WO2003055337A1 (en) | 2001-12-21 | 2002-12-23 | Improvements relating to smokable filler materials |
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| EP (1) | EP1460908B1 (en) |
| JP (1) | JP2005512585A (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4625737A (en) * | 1982-12-30 | 1986-12-02 | Philip Morris Incorporated | Foamed, extruded, tobacco-containing smoking article and method of making the same |
| US4611608A (en) * | 1984-01-13 | 1986-09-16 | Naarden International N.V. | Process for utilizing tobacco dust |
| GB8704196D0 (en) * | 1987-02-23 | 1987-04-01 | British American Tobacco Co | Tobacco reconstitution |
| GB0011351D0 (en) * | 2000-05-12 | 2000-06-28 | British American Tobacco Co | Tobacco reconstitution |
-
2001
- 2001-12-21 GB GBGB0130627.3A patent/GB0130627D0/en not_active Ceased
-
2002
- 2002-12-23 MX MXPA04006160A patent/MXPA04006160A/en not_active Application Discontinuation
- 2002-12-23 CN CNA028279638A patent/CN1617680A/en active Pending
- 2002-12-23 AT AT02791917T patent/ATE361002T1/en not_active IP Right Cessation
- 2002-12-23 DE DE60219956T patent/DE60219956D1/en not_active Expired - Lifetime
- 2002-12-23 AU AU2002358221A patent/AU2002358221B2/en not_active Ceased
- 2002-12-23 WO PCT/GB2002/005899 patent/WO2003055337A1/en active IP Right Grant
- 2002-12-23 KR KR10-2004-7009628A patent/KR20040068292A/en not_active Application Discontinuation
- 2002-12-23 CA CA002469917A patent/CA2469917A1/en not_active Abandoned
- 2002-12-23 JP JP2003555918A patent/JP2005512585A/en not_active Ceased
- 2002-12-23 RU RU2004122619/12A patent/RU2293502C2/en not_active IP Right Cessation
- 2002-12-23 BR BR0215208-8A patent/BR0215208A/en not_active IP Right Cessation
- 2002-12-23 EP EP02791917A patent/EP1460908B1/en not_active Expired - Lifetime
- 2002-12-23 US US10/499,553 patent/US20050098187A1/en not_active Abandoned
-
2004
- 2004-07-21 ZA ZA200405835A patent/ZA200405835B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| AU2002358221B2 (en) | 2006-10-26 |
| EP1460908B1 (en) | 2007-05-02 |
| GB0130627D0 (en) | 2002-02-06 |
| ZA200405835B (en) | 2005-10-21 |
| RU2293502C2 (en) | 2007-02-20 |
| WO2003055337A1 (en) | 2003-07-10 |
| US20050098187A1 (en) | 2005-05-12 |
| DE60219956D1 (en) | 2007-06-14 |
| RU2004122619A (en) | 2005-08-10 |
| EP1460908A1 (en) | 2004-09-29 |
| ATE361002T1 (en) | 2007-05-15 |
| CN1617680A (en) | 2005-05-18 |
| JP2005512585A (en) | 2005-05-12 |
| BR0215208A (en) | 2004-10-26 |
| CA2469917A1 (en) | 2003-07-10 |
| MXPA04006160A (en) | 2004-11-01 |
| KR20040068292A (en) | 2004-07-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FGA | Letters patent sealed or granted (standard patent) | ||
| MK14 | Patent ceased section 143(a) (annual fees not paid) or expired |