EP4064866B1 - Aerosol-generating material comprising an amorphous solid comprising methol and calcium-crosslinked alginate - Google Patents
Aerosol-generating material comprising an amorphous solid comprising methol and calcium-crosslinked alginate Download PDFInfo
- Publication number
- EP4064866B1 EP4064866B1 EP20816936.7A EP20816936A EP4064866B1 EP 4064866 B1 EP4064866 B1 EP 4064866B1 EP 20816936 A EP20816936 A EP 20816936A EP 4064866 B1 EP4064866 B1 EP 4064866B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- aerosol
- generating material
- amorphous solid
- article
- menthol
- 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.)
- Active
Links
- 239000000463 material Substances 0.000 title claims description 212
- 239000007787 solid Substances 0.000 title claims description 140
- 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 title claims description 34
- 235000010443 alginic acid Nutrition 0.000 title claims description 34
- 229920000615 alginic acid Polymers 0.000 title claims description 34
- 229940072056 alginate Drugs 0.000 title claims description 32
- 239000000443 aerosol Substances 0.000 claims description 116
- 238000010438 heat treatment Methods 0.000 claims description 64
- 239000002002 slurry Substances 0.000 claims description 45
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims description 42
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 42
- 229940041616 menthol Drugs 0.000 claims description 42
- 239000003349 gelling agent Substances 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 27
- 239000011575 calcium Substances 0.000 claims description 23
- 229910052791 calcium Inorganic materials 0.000 claims description 23
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 19
- 235000010987 pectin Nutrition 0.000 claims description 18
- 229920001277 pectin Polymers 0.000 claims description 18
- 239000001814 pectin Substances 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 16
- -1 Ca2+ cations Chemical class 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008365 aqueous carrier Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- IAJILQKETJEXLJ-SQOUGZDYSA-N L-guluronic acid Chemical compound O=C[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O IAJILQKETJEXLJ-SQOUGZDYSA-N 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 6
- AEMOLEFTQBMNLQ-VANFPWTGSA-N D-mannopyranuronic acid Chemical compound OC1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-VANFPWTGSA-N 0.000 claims description 5
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 claims description 2
- 239000004386 Erythritol Substances 0.000 claims 1
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 claims 1
- 229940009714 erythritol Drugs 0.000 claims 1
- 235000019414 erythritol Nutrition 0.000 claims 1
- 238000001816 cooling Methods 0.000 description 60
- 238000009423 ventilation Methods 0.000 description 34
- 241000208125 Nicotiana Species 0.000 description 30
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 30
- 239000000123 paper Substances 0.000 description 25
- 239000010410 layer Substances 0.000 description 22
- 229960005069 calcium Drugs 0.000 description 17
- 239000000499 gel Substances 0.000 description 17
- 239000000945 filler Substances 0.000 description 12
- 239000011888 foil Substances 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 11
- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 description 10
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 description 10
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 description 10
- 229950011318 cannabidiol Drugs 0.000 description 10
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 description 10
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 9
- 239000000796 flavoring agent Substances 0.000 description 9
- 229960002715 nicotine Drugs 0.000 description 9
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 9
- 230000006698 induction Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 7
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 7
- 239000001527 calcium lactate Substances 0.000 description 7
- 235000011086 calcium lactate Nutrition 0.000 description 7
- 229960002401 calcium lactate Drugs 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000391 smoking effect Effects 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- CYQFCXCEBYINGO-UHFFFAOYSA-N THC Natural products C1=C(C)CCC2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3C21 CYQFCXCEBYINGO-UHFFFAOYSA-N 0.000 description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 6
- 235000010980 cellulose Nutrition 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- CYQFCXCEBYINGO-IAGOWNOFSA-N delta1-THC Chemical compound C1=C(C)CC[C@H]2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3[C@@H]21 CYQFCXCEBYINGO-IAGOWNOFSA-N 0.000 description 6
- 229960004242 dronabinol Drugs 0.000 description 6
- 239000012212 insulator Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 229920002301 cellulose acetate Polymers 0.000 description 5
- 238000003780 insertion Methods 0.000 description 5
- 230000037431 insertion Effects 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 230000001953 sensory effect Effects 0.000 description 5
- 235000010413 sodium alginate Nutrition 0.000 description 5
- 239000000661 sodium alginate Substances 0.000 description 5
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 4
- AAXZFUQLLRMVOG-UHFFFAOYSA-N 2-methyl-2-(4-methylpent-3-enyl)-7-propylchromen-5-ol Chemical compound C1=CC(C)(CCC=C(C)C)OC2=CC(CCC)=CC(O)=C21 AAXZFUQLLRMVOG-UHFFFAOYSA-N 0.000 description 4
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 description 4
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 229920002907 Guar gum Polymers 0.000 description 4
- 229920000084 Gum arabic Polymers 0.000 description 4
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 4
- 235000010489 acacia gum Nutrition 0.000 description 4
- 239000000205 acacia gum Substances 0.000 description 4
- 235000010216 calcium carbonate Nutrition 0.000 description 4
- 239000004281 calcium formate Substances 0.000 description 4
- 229940044172 calcium formate Drugs 0.000 description 4
- 235000019255 calcium formate Nutrition 0.000 description 4
- 159000000007 calcium salts Chemical class 0.000 description 4
- 239000002775 capsule Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000002657 fibrous material Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 239000000665 guar gum Substances 0.000 description 4
- 235000010417 guar gum Nutrition 0.000 description 4
- 229960002154 guar gum Drugs 0.000 description 4
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 4
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 4
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 4
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 4
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 4
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 230000035515 penetration Effects 0.000 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 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000005711 Benzoic acid Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 235000010233 benzoic acid Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 235000011148 calcium chloride Nutrition 0.000 description 3
- 239000011111 cardboard Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 3
- 230000001976 improved effect Effects 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 229940005550 sodium alginate Drugs 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 2
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 2
- RBEAVAMWZAJWOI-MTOHEIAKSA-N (5as,6s,9r,9ar)-6-methyl-3-pentyl-9-prop-1-en-2-yl-7,8,9,9a-tetrahydro-5ah-dibenzofuran-1,6-diol Chemical compound C1=2C(O)=CC(CCCCC)=CC=2O[C@H]2[C@@H]1[C@H](C(C)=C)CC[C@]2(C)O RBEAVAMWZAJWOI-MTOHEIAKSA-N 0.000 description 2
- ZROLHBHDLIHEMS-HUUCEWRRSA-N (6ar,10ar)-6,6,9-trimethyl-3-propyl-6a,7,8,10a-tetrahydrobenzo[c]chromen-1-ol Chemical compound C1=C(C)CC[C@H]2C(C)(C)OC3=CC(CCC)=CC(O)=C3[C@@H]21 ZROLHBHDLIHEMS-HUUCEWRRSA-N 0.000 description 2
- IXJXRDCCQRZSDV-GCKMJXCFSA-N (6ar,9r,10as)-6,6,9-trimethyl-3-pentyl-6a,7,8,9,10,10a-hexahydro-6h-1,9-epoxybenzo[c]chromene Chemical compound C1C[C@@H](C(O2)(C)C)[C@@H]3C[C@]1(C)OC1=C3C2=CC(CCCCC)=C1 IXJXRDCCQRZSDV-GCKMJXCFSA-N 0.000 description 2
- YJYIDZLGVYOPGU-XNTDXEJSSA-N 2-[(2e)-3,7-dimethylocta-2,6-dienyl]-5-propylbenzene-1,3-diol Chemical compound CCCC1=CC(O)=C(C\C=C(/C)CCC=C(C)C)C(O)=C1 YJYIDZLGVYOPGU-XNTDXEJSSA-N 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 2
- KASVLYINZPAMNS-UHFFFAOYSA-N Cannabigerol monomethylether Natural products CCCCCC1=CC(O)=C(CC=C(C)CCC=C(C)C)C(OC)=C1 KASVLYINZPAMNS-UHFFFAOYSA-N 0.000 description 2
- 229920008347 Cellulose acetate propionate Polymers 0.000 description 2
- UCONUSSAWGCZMV-HZPDHXFCSA-N Delta(9)-tetrahydrocannabinolic acid Chemical compound C([C@H]1C(C)(C)O2)CC(C)=C[C@H]1C1=C2C=C(CCCCC)C(C(O)=O)=C1O UCONUSSAWGCZMV-HZPDHXFCSA-N 0.000 description 2
- ZROLHBHDLIHEMS-UHFFFAOYSA-N Delta9 tetrahydrocannabivarin Natural products C1=C(C)CCC2C(C)(C)OC3=CC(CCC)=CC(O)=C3C21 ZROLHBHDLIHEMS-UHFFFAOYSA-N 0.000 description 2
- VZWGRQBCURJOMT-UHFFFAOYSA-N Dodecyl acetate Chemical compound CCCCCCCCCCCCOC(C)=O VZWGRQBCURJOMT-UHFFFAOYSA-N 0.000 description 2
- MWAYRGBWOVHDDZ-UHFFFAOYSA-N Ethyl vanillate Chemical compound CCOC(=O)C1=CC=C(O)C(OC)=C1 MWAYRGBWOVHDDZ-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- UYXTWWCETRIEDR-UHFFFAOYSA-N Tributyrin Chemical compound CCCC(=O)OCC(OC(=O)CCC)COC(=O)CCC UYXTWWCETRIEDR-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 235000010419 agar Nutrition 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 229960001126 alginic acid Drugs 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 2
- 235000010407 ammonium alginate Nutrition 0.000 description 2
- 239000000728 ammonium alginate Substances 0.000 description 2
- 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 2
- 230000008901 benefit Effects 0.000 description 2
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 description 2
- 235000019437 butane-1,3-diol Nutrition 0.000 description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 2
- 239000001639 calcium acetate Substances 0.000 description 2
- 229960005147 calcium acetate Drugs 0.000 description 2
- 235000011092 calcium acetate Nutrition 0.000 description 2
- FNAQSUUGMSOBHW-UHFFFAOYSA-H calcium citrate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FNAQSUUGMSOBHW-UHFFFAOYSA-H 0.000 description 2
- 239000001354 calcium citrate Substances 0.000 description 2
- 229960004256 calcium citrate Drugs 0.000 description 2
- YJYIDZLGVYOPGU-UHFFFAOYSA-N cannabigeroldivarin Natural products CCCC1=CC(O)=C(CC=C(C)CCC=C(C)C)C(O)=C1 YJYIDZLGVYOPGU-UHFFFAOYSA-N 0.000 description 2
- 229930003827 cannabinoid Natural products 0.000 description 2
- 239000003557 cannabinoid Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 235000010418 carrageenan Nutrition 0.000 description 2
- 239000000679 carrageenan Substances 0.000 description 2
- 229920001525 carrageenan Polymers 0.000 description 2
- 229940113118 carrageenan Drugs 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- ZDJFDFNNEAPGOP-UHFFFAOYSA-N dimethyl tetradecanedioate Chemical compound COC(=O)CCCCCCCCCCCCC(=O)OC ZDJFDFNNEAPGOP-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000007787 electrohydrodynamic spraying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- MMXKVMNBHPAILY-UHFFFAOYSA-N ethyl laurate Chemical compound CCCCCCCCCCCC(=O)OCC MMXKVMNBHPAILY-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 229940040102 levulinic acid Drugs 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012766 organic filler Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 235000010408 potassium alginate Nutrition 0.000 description 2
- 239000000737 potassium alginate Substances 0.000 description 2
- 235000013772 propylene glycol Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 2
- 235000013337 tricalcium citrate Nutrition 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- 235000010493 xanthan gum Nutrition 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 229940082509 xanthan gum Drugs 0.000 description 2
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical group CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 244000215068 Acacia senegal Species 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920000936 Agarose Polymers 0.000 description 1
- 229910017083 AlN Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- UVOLYTDXHDXWJU-UHFFFAOYSA-N Cannabichromene Chemical compound C1=CC(C)(CCC=C(C)C)OC2=CC(CCCCC)=CC(O)=C21 UVOLYTDXHDXWJU-UHFFFAOYSA-N 0.000 description 1
- REOZWEGFPHTFEI-JKSUJKDBSA-N Cannabidivarin Chemical compound OC1=CC(CCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 REOZWEGFPHTFEI-JKSUJKDBSA-N 0.000 description 1
- VBGLYOIFKLUMQG-UHFFFAOYSA-N Cannabinol Chemical compound C1=C(C)C=C2C3=C(O)C=C(CCCCC)C=C3OC(C)(C)C2=C1 VBGLYOIFKLUMQG-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- AEMOLEFTQBMNLQ-BZINKQHNSA-N D-Guluronic Acid Chemical compound OC1O[C@H](C(O)=O)[C@H](O)[C@@H](O)[C@H]1O AEMOLEFTQBMNLQ-BZINKQHNSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000004348 Glyceryl diacetate Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229920000161 Locust bean gum Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- IGHTZQUIFGUJTG-QSMXQIJUSA-N O1C2=CC(CCCCC)=CC(O)=C2[C@H]2C(C)(C)[C@@H]3[C@H]2[C@@]1(C)CC3 Chemical compound O1C2=CC(CCCCC)=CC(O)=C2[C@H]2C(C)(C)[C@@H]3[C@H]2[C@@]1(C)CC3 IGHTZQUIFGUJTG-QSMXQIJUSA-N 0.000 description 1
- MIYFJEKZLFWKLZ-UHFFFAOYSA-N Phenylmethyl benzeneacetate Chemical compound C=1C=CC=CC=1COC(=O)CC1=CC=CC=C1 MIYFJEKZLFWKLZ-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004373 Pullulan Substances 0.000 description 1
- 229920001218 Pullulan Polymers 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N Tetraethylene glycol, Natural products OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229940061720 alpha hydroxy acid Drugs 0.000 description 1
- 150000001280 alpha hydroxy acids Chemical class 0.000 description 1
- 150000004716 alpha keto acids Chemical class 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 229960002903 benzyl benzoate Drugs 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229960003563 calcium carbonate Drugs 0.000 description 1
- 229960002713 calcium chloride Drugs 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- WVOLTBSCXRRQFR-DLBZAZTESA-N cannabidiolic acid Chemical compound OC1=C(C(O)=O)C(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 WVOLTBSCXRRQFR-DLBZAZTESA-N 0.000 description 1
- QXACEHWTBCFNSA-SFQUDFHCSA-N cannabigerol Chemical compound CCCCCC1=CC(O)=C(C\C=C(/C)CCC=C(C)C)C(O)=C1 QXACEHWTBCFNSA-SFQUDFHCSA-N 0.000 description 1
- SVTKBAIRFMXQQF-UHFFFAOYSA-N cannabivarin Chemical compound C1=C(C)C=C2C3=C(O)C=C(CCC)C=C3OC(C)(C)C2=C1 SVTKBAIRFMXQQF-UHFFFAOYSA-N 0.000 description 1
- 235000013736 caramel Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000007942 carboxylates Chemical group 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- HKQOBOMRSSHSTC-UHFFFAOYSA-N cellulose acetate Chemical compound OC1C(O)C(O)C(CO)OC1OC1C(CO)OC(O)C(O)C1O.CC(=O)OCC1OC(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(COC(C)=O)O1.CCC(=O)OCC1OC(OC(=O)CC)C(OC(=O)CC)C(OC(=O)CC)C1OC1C(OC(=O)CC)C(OC(=O)CC)C(OC(=O)CC)C(COC(=O)CC)O1 HKQOBOMRSSHSTC-UHFFFAOYSA-N 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019506 cigar Nutrition 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- PEUGOJXLBSIJQS-UHFFFAOYSA-N diethyl octanedioate Chemical compound CCOC(=O)CCCCCCC(=O)OCC PEUGOJXLBSIJQS-UHFFFAOYSA-N 0.000 description 1
- IZMOTZDBVPMOFE-UHFFFAOYSA-N dimethyl dodecanedioate Chemical compound COC(=O)CCCCCCCCCCC(=O)OC IZMOTZDBVPMOFE-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 1
- 150000007520 diprotic acids Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003571 electronic cigarette Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012765 fibrous filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011087 fumaric acid Nutrition 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 235000019443 glyceryl diacetate Nutrition 0.000 description 1
- 239000001087 glyceryl triacetate Substances 0.000 description 1
- 235000013773 glyceryl triacetate Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011084 greaseproof paper Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000000416 hydrocolloid Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 235000010420 locust bean gum Nutrition 0.000 description 1
- 239000000711 locust bean gum Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 150000007518 monoprotic acids Chemical class 0.000 description 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 1
- 239000000978 natural dye Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000004804 polysaccharides Chemical class 0.000 description 1
- 229920001296 polysiloxane Chemical class 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 229940107700 pyruvic acid Drugs 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 235000019794 sodium silicate Nutrition 0.000 description 1
- 239000008275 solid aerosol Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000000979 synthetic dye Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
- 150000003627 tricarboxylic acid derivatives Chemical class 0.000 description 1
- 239000001069 triethyl citrate Substances 0.000 description 1
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
- 235000013769 triethyl citrate Nutrition 0.000 description 1
- 150000007521 triprotic acids Chemical class 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
-
- 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
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- 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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
-
- 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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
-
- 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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/32—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by acyclic compounds
-
- 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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/34—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances containing a carbocyclic ring other than a six-membered aromatic ring
-
- 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
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/42—Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D1/00—Cigars; Cigarettes
- A24D1/20—Cigarettes specially adapted for simulated smoking devices
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/20—Devices using solid inhalable precursors
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
- A24F40/46—Shape or structure of electric heating means
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/50—Control or monitoring
- A24F40/57—Temperature control
Definitions
- the present invention relates to aerosol generation.
- Smoking articles such as cigarettes, cigars and the like burn tobacco during use to create tobacco smoke.
- Alternatives to these types of articles release an inhalable aerosol or vapour by releasing compounds from a substrate material by heating without burning. These may be referred to as non-combustible smoking articles or aerosol generating assemblies.
- a heating device which release compounds by heating, but not burning, a solid aerosol-generating material.
- This solid aerosol-generating material may, in some cases, contain a tobacco material.
- the heating volatilises at least one component of the material, typically forming an inhalable aerosol.
- These products may be referred to as heat-not-burn devices, tobacco heating devices or tobacco heating products.
- Various different arrangements for volatilising at least one component of the solid aerosol-generating material are known.
- e-cigarette / tobacco heating product hybrid devices also known as electronic tobacco hybrid devices.
- These hybrid devices contain a liquid source (which may or may not contain nicotine) which is vaporised by heating to produce an inhalable vapour or aerosol.
- the device additionally contains a solid aerosol-generating material (which may or may not contain a tobacco material) and components of this material are entrained in the inhalable vapour or aerosol to produce the inhaled medium.
- US 2011/104218 describes capsules for smoking articles prepared by forming hydrogel capsules of specific diameter with at least one coating layer.
- WO 2014/083333 describes a smokable material having a controlled filling value.
- WO 2011/117748 describes a method for providing an encapsulated flavourant and/or chemesthetic agent in a smoking article.
- WO 2016/184977 describes a solid aerosol generating material that comprises about 5-35 wt% tobacco extract, about 50-80 wt% filler, about 10-35 wt% aerosol generating agent and about 2.5-10 wt% binder.
- WO 2005/058078 describes a smoking article comprising discrete segments of smokable material having an encapsulated flavourant contained within a component of the smokable material.
- an aerosol-generating material comprising an amorphous solid, the amorphous solid comprising:
- a substrate comprising an aerosol-generating material as described herein and a support on which the aerosol-generating material is provided.
- an article for use with a non-combustible aerosol provision device comprising an aerosol-generating material as described herein and/or a substrate as described herein.
- a non-combustible aerosol provision system comprising an article as described herein and a non-combustible aerosol provision device, wherein the non-combustible aerosol provision device is configured to generate aerosol from the article when the article is used with the non-combustible aerosol provision device, wherein the non-combustible aerosol provision device comprises a heater configured to heat but not burn the article.
- a method of generating an aerosol using a non-combustible aerosol provision system as described herein comprising heating the aerosol-generating material.
- the method comprises heating the aerosol-generating material to a temperature of less than 350 °C.
- the method comprises heating the aerosol-generating material to a temperature of from about 220 °C to about 280 °C.
- Aerosol-generating material described herein is material that is capable of generating aerosol, for example when heated, irradiated or energized in any other way.
- Aerosol-generating material may, for example, be in the form of a solid, liquid or gel which may or may not contain nicotine and/or flavourants.
- the aerosol-generating material comprises an "amorphous solid", which may alternatively be referred to as a "monolithic solid” (i.e. non-fibrous).
- the amorphous solid may be a dried gel.
- the amorphous solid is a solid material that may retain some fluid, such as liquid, within it.
- the aerosol-generating material may for example comprise from about 50wt%, 60wt% or 70wt% of amorphous solid, to about 90wt%, 95wt% or 100wt% of amorphous solid. In some cases, the aerosol generating material consists of amorphous solid.
- the invention provides aerosol-generating material comprising an amorphous solid, the amorphous solid comprising:
- the gelling agent of the present invention comprises alginate salts (also referred to as "alginate").
- Alginate salts are derivatives of alginic acid, and are linear polysaccharides comprising G units and typically M units. On addition of divalent cations to alginic acid, the alginate crosslinks to form a gel.
- G unit refers to ⁇ -(1-4)-linked L-guluronate.
- ⁇ -L-guluronate is the conjugate base of ⁇ -L-guluronic acid.
- a G unit may also be referred to as a guluronate momomer, or a G residue.
- M unit refers to ⁇ -(1-4)-linked D-mannuronate.
- ⁇ -D-mannuronate is the conjugate base of ⁇ -D-mannuronic acid.
- An M unit may also be referred to as a mannuronate monomer, or an M residue.
- Divalent cations such as Ca 2+ interact with the carboxylate groups of the alginate monomers to form ionic crosslinks; the amorphous solid of the present invention comprises calcium-crosslinked alginate.
- the inventors have established that the physical characteristics of an amorphous solid comprising calcium-crosslinked alginate depends on the molar ratio of calcium cations (Ca 2+ ) to, in particular, the alginate G units in the amorphous solid.
- the amorphous solid of the present invention comprises menthol.
- Menthol is present in the amorphous solid as an active substance. That is, menthol is included in the amorphous solid such that, upon heating of the amorphous solid, menthol is aerosolised and may be delivered to a user in order to achieve a physiological and/or olfactory response.
- menthol Due to the physical characteristics of menthol (e.g. its volatility, solubility and so on), it is difficult to provide a menthol-containing amorphous solid which has an acceptable shelf-life and delivers an acceptable inhalable aerosol to a user when heated in a non-combustible aerosol provision system.
- the amorphous solid should retain a desirable amount of menthol during storage until the point at which the amorphous solid heated in a non-combustible aerosol provision system.
- the amorphous solid should be configured to release a desirable amount of menthol as part of an inhalable aerosol upon heating of the amorphous solid.
- the present inventors have identified that configuring the amorphous solid such that the molar ratio of Ca 2+ to G units in the alginate is from 0.2 to 1 provides a menthol-containing aerosol-generating material which has a good shelf-life and also releases a desirable amount of menthol upon heating of the aerosol-generating material in a non-combustible aerosol provision device.
- the molar ratio of Ca 2+ to G units in the alginate is from 0.3:1 to 0.5:1.
- the molar ratio of Ca 2+ to G units in the alginate is approximately 0.4:1 ("approximately" allowing for a 20% tolerance).
- an amorphous solid having a Ca 2+ content higher than that of the present invention would result in syneresis and thus deterioration of the aerosol-generating material during storage, and an amorphous solid having a Ca 2+ content lower than that of the present invention would not retain a desirable amount of menthol after storage.
- the calcium-crosslinked alginate comprises a combination of G units and M units.
- the G units and M units are present in a molar ratio of from 1:2 to 10:1 (i.e. the number of ⁇ -(1-4)-linked L-guluronate units present compared with the number of ( ⁇ -(1-4)-linked D-mannuronate units).
- the G units and M units are present in a molar ratio of from 1:3 to 3:1, or from 1:2 to 2:1, or from 1:1.5 to 1.5:1, or from 1:1.2 to 1.2:1.
- the aerosol-generating material when stored for 30 days in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- the aerosol-generating material when stored for 6 weeks (42 days) in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- the aerosol-generating material when stored for 16 weeks (112 days) in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- alginate is comprised in the gelling agent in an amount of from 15-40wt% of the amorphous solid. That is, the amorphous solid comprises alginate in an amount of 15-40wt% by dry weight of the amorphous solid. In some embodiments, the amorphous solid comprises alginate in an amount of from 10-35wt%, or 15wt% to 30wt%.
- the gelling agent further comprises pectin.
- the alginate and pectin are present in a ratio of alginate to pectin of from 1:1 to 10:1. In some embodiments, the ratio of alginate to pectin is from 3:1 to 8:1, or 5:1 to 7: 1.The ratio of alginate to pectin is expressed as a dry weight ratio (w/w).
- a gelling agent comprising alginate and pectin in such ratios may provide an improved amorphous solid.
- a combination of alginate and pectin may have a synergistic effect on the binding in the amorphous solid.
- combining alginate and pectin in particular ratios may influence the temperature at which menthol is released from the amorphous solid when heated.
- Providing a gelling agent which comprises more alginate than pectin may be advantageous due to lower material costs.
- a gelling agent comprising alginate alone may have a high viscosity, meaning that it is difficult to process the gelling agent during the manufacture of the amorphous solid.
- the inventors have identified that, by combining alginate with pectin wherein pectin is present as a minority portion, the viscosity of the gelling agent may be easier to process during the manufacture of the amorphous solid.
- the pectin is comprised in the gelling agent in an amount of from 3-10wt% of the amorphous solid. That is, the amorphous solid comprises pectin in an amount of 3-10wt% by dry weight of the amorphous solid. In some embodiments, the amorphous solid comprises pectin in an amount of from 3-8wt%, or 4wt% to 6wt%.
- the amorphous solid comprises from about 1wt%, 5wt%, 10wt%, 15wt%, 20wt% or 25wt% to about 60wt%, 50wt%, 45wt%, 40wt%, 35wt%, 30wt% or 27wt% of gelling agent (all calculated on a dry weight basis).
- the amorphous solid may comprise 1-50wt%, 5-40wt%, or 25-3 5wt% of a gelling agent.
- the gelling agent further comprises a hydrocolloid other than those mentioned above.
- the gelling agent further comprises one or more compounds selected from the group comprising starches (and derivatives), celluloses (and derivatives, such as such as methylcellulose, hydroxypropyl cellulose, and carboxymethyl cellulose (CMC)), gums, silica or silicones compounds, clays, polyvinyl alcohol and combinations thereof.
- the gelling agent further comprises one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose, pullulan, xanthan gum, guar gum, carrageenan, agarose, acacia gum, fumed silica, PDMS, sodium silicate, kaolin and polyvinyl alcohol.
- the gelling agent may further comprise one or more compounds selected from cellulosic gelling agents, non-cellulosic gelling agents, guar gum, acacia gum and mixtures thereof.
- the cellulosic gelling agent is selected from the group consisting of: hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose (CMC), hydroxypropyl methylcellulose (HPMC), methyl cellulose, ethyl cellulose, cellulose acetate (CA), cellulose acetate butyrate (CAB), cellulose acetate propionate (CAP) and combinations thereof.
- the gelling agent further comprises one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose (HPMC), carboxymethylcellulose, guar gum, or acacia gum.
- the gelling agent further comprises one or more non-cellulosic gelling agents, including, but not limited to, agar, xanthan gum, gum Arabic, guar gum, locust bean gum, carrageenan, starch, and combinations thereof.
- the non-cellulose based gelling agent further comprises agar.
- the aerosol-generating material comprises menthol in an amount of from 0.1-80wt%. In some embodiments, the aerosol-generating material comprises menthol in an amount of from about 1wt%, 5wt%, 10wt%, 15wt%, 20wt% or 25wt% to about 70wt%, 50wt%, 45wt% or 40wt% (calculated on a dry weight basis). In particular embodiments, the amorphous solid comprises 10-60wt%, 40-60wt% or 45-55wt% of menthol.
- the amorphous solid comprises 0.1-50wt% aerosol-former material. In some embodiments, the amorphous solid comprises 10-30wt% aerosol-former material, or 15-25wt% aerosol-former material.
- the aerosol-former material may comprise one or more of glycerine, glycerol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,3-butylene glycol, erythritol, meso-Erythritol, ethyl vanillate, ethyl laurate, a diethyl suberate, triethyl citrate, triacetin, a diacetin mixture, benzyl benzoate, benzyl phenyl acetate, tributyrin, lauryl acetate, lauric acid, myristic acid, and propylene carbonate.
- the aerosol former comprises one or more polyhydric alcohols, such as propylene glycol, triethylene glycol, 1 ,3-butanediol and glycerin; esters of polyhydric alcohols, such as glycerol mono-, di- or triacetate; and/or aliphatic esters of mono-, di- or polycarboxylic acids, such as dimethyl dodecanedioate and dimethyl tetradecanedioate.
- polyhydric alcohols such as propylene glycol, triethylene glycol, 1 ,3-butanediol and glycerin
- esters of polyhydric alcohols such as glycerol mono-, di- or triacetate
- aliphatic esters of mono-, di- or polycarboxylic acids such as dimethyl dodecanedioate and dimethyl tetradecanedioate.
- the amorphous solid comprises:
- the amorphous solid may have any suitable water content, such as from 1wt% to 15wt% (wet weight basis - "WWB").
- WWB wet weight basis -
- the water content of the amorphous solid may be from about 5wt%, 7wt% or 9wt% to about 15wt%, 13wt% or 11wt% (WWB).
- the aerosolisable or non-aerosol-generating material may be present on or in a support to form a substrate.
- the support functions as a support on which the amorphous solid layer forms, easing manufacture.
- the support may provide rigidity to the amorphous solid layer, easing handling.
- the support may be any suitable material which can be used to support an amorphous solid.
- the support may be formed from materials selected from metal foil, paper, carbon paper, greaseproof paper, ceramic, carbon allotropes such as graphite and graphene, plastic, cardboard, wood or combinations thereof.
- the support may comprise or consist of a tobacco material, such as a sheet of reconstituted tobacco.
- the support may be formed from materials selected from metal foil, paper, cardboard, wood or combinations thereof.
- the support comprises paper.
- the support itself be a laminate structure comprising layers of materials selected from the preceding lists.
- the support may also function as a flavour support.
- the support may be impregnated with a flavourant or with tobacco extract.
- the thickness of the support layer may be in the range of about 10 ⁇ m, 15 ⁇ m, 17 ⁇ m, 20 ⁇ m, 23 ⁇ m, 25 ⁇ m, 50 ⁇ m, 75 ⁇ m or 0.1mm to about 2.5mm, 2.0mm, 1.5mm, 1.0mm or 0.5mm.
- the support may comprise more than one layer, and the thickness described herein refers to the aggregate thickness of those layers.
- the support may be magnetic. This functionality may be used to fasten the support to the assembly in use, or may be used to generate particular amorphous solid shapes.
- the aerosol generating substrate may comprise one or more magnets which can be used to fasten the substrate to an induction heater in use.
- the support may be substantially or wholly impermeable to gas and/or aerosol. This prevents aerosol or gas passage through the support layer, thereby controlling the flow and ensuring it is delivered to the user. This can also be used to prevent condensation or other deposition of the gas/aerosol in use on, for example, the surface of a heater provided in an aerosol generating assembly. Thus, consumption efficiency and hygiene can be improved in some cases.
- the surface of the support that abuts the amorphous solid may be porous.
- the support comprises paper.
- a porous support such as paper is particularly suitable for the present invention; the porous (e.g. paper) layer abuts the amorphous solid layer and forms a strong bond.
- the amorphous solid is formed by drying a gel and, without being limited by theory, it is thought that the slurry from which the gel is formed partially impregnates the porous support (e.g. paper) so that when the gel sets and forms cross-links, the support is partially bound into the gel. This provides a strong binding between the gel and the support (and between the dried gel and the support).
- surface roughness may contribute to the strength of bond between the amorphous material and the support.
- the inventors have found that the paper roughness (for the surface abutting the support) may suitably be in the range of 50-1000 Bekk seconds, suitably 50-150 Bekk seconds, suitably 100 Bekk seconds (measured over an air pressure interval of 50.66-48.00 kPa).
- a Bekk smoothness tester is an instrument used to determine the smoothness of a paper surface, in which air at a specified pressure is leaked between a smooth glass surface and a paper sample, and the time (in seconds) for a fixed volume of air to seep between these surfaces is the "Bekk smoothness".
- the surface of the support facing away from the amorphous solid may be arranged in contact with the heater, and a smoother surface may provide more efficient heat transfer.
- the support is disposed so as to have a rougher side abutting the amorphous material and a smoother side facing away from the amorphous material.
- the support may be a paper-backed foil; the paper layer abuts the amorphous solid layer and the properties discussed in the previous paragraphs are afforded by this abutment.
- the foil backing is substantially impermeable, providing control of the aerosol flow path.
- a metal foil backing may also serve to conduct heat to the amorphous solid.
- the foil layer of the paper-backed foil abuts the amorphous solid.
- the foil is substantially impermeable, thereby preventing water provided in the amorphous solid to be absorbed into the paper which could weaken its structural integrity.
- the support is formed from or comprises metal foil, such as aluminium foil.
- a metallic support may allow for better conduction of thermal energy to the amorphous solid.
- a metal foil may function as a susceptor in an induction heating system.
- the support comprises a metal foil layer and a support layer, such as cardboard.
- the metal foil layer may have a thickness of less than 20 ⁇ m, such as from about 1 ⁇ m to about 10 ⁇ m, suitably about 5 ⁇ m.
- the support may have a thickness of between about 0.017mm and about 2.0mm, suitably from about 0.02mm, 0.05mm or 0.1mm to about 1.5mm, 1.0mm, or 0.5mm.
- the aerosol generating substrate may comprise embedded heating means, such as resistive or inductive heating elements.
- the heating means may be embedded in the amorphous solid.
- the amorphous solid may be made from a gel, and this gel may additionally comprise a solvent, included at 0.1-50wt%.
- a solvent in which the flavour is soluble may reduce the gel stability and the flavour may crystallise out of the gel.
- the gel does not include a solvent in which the flavour is soluble.
- the amorphous solid comprises less than 60wt% of a filler, such as from 1wt% to 60wt%, or 5wt% to 50wt%, or 5wt% to 30wt%, or 10wt% to 20wt%.
- the amorphous solid comprises less than 20wt%, suitably less than 10wt% or less than 5wt% of a filler. In some cases, the amorphous solid comprises less than 1wt% of a filler, and in some cases, comprises no filler.
- a consumable is an article, part or all of which is intended to be consumed during use by a user.
- a consumable may comprise or consist of aerosol-generating material.
- a consumable may comprise one or more other elements, such as a filter or an aerosol modifying substance.
- a consumable may comprise a heating element that emits heat to cause the aerosol-generating material to generate aerosol in use.
- the heating element may, for example, comprise combustible material, or may comprise a susceptor that is heatable by penetration with a varying magnetic field.
- Articles of the present invention may be provided in any suitable shape.
- the article is provided as a rod (e.g. substantially cylindrical).
- An article provided as a rod may include the aerosol-generating material as a shredded sheet, optionally blended with cut tobacco.
- the article provided as a rod may include the aerosol-generating material as a sheet, such as a sheet circumscribing a rod of aerosol-generating material (e.g. tobacco).
- the article comprises a layer portion of aerosol-generating material disposed on a carrier.
- the article may have at least one substantially planar (flat) surface.
- a susceptor is material that is heatable by penetration with a varying magnetic field, such as an alternating magnetic field.
- the heating material may be an electrically-conductive material, so that penetration thereof with a varying magnetic field causes induction heating of the heating material.
- the heating material may be magnetic material, so that penetration thereof with a varying magnetic field causes magnetic hysteresis heating of the heating material.
- the heating material may be both electrically-conductive and magnetic, so that the heating material is heatable by both heating mechanisms.
- Induction heating is a process in which an electrically-conductive object is heated by penetrating the object with a varying magnetic field.
- An induction heater may comprise an electromagnet and a device for passing a varying electrical current, such as an alternating current, through the electromagnet.
- a varying electrical current such as an alternating current
- the electromagnet and the object to be heated are suitably relatively positioned so that the resultant varying magnetic field produced by the electromagnet penetrates the object, one or more eddy currents are generated inside the object.
- the object has a resistance to the flow of electrical currents. Therefore, when such eddy currents are generated in the object, their flow against the electrical resistance of the object causes the obj ect to be heated. This process is called Joule, ohmic, or resistive heating.
- the susceptor is in the form of a closed circuit. It has been found that, when the susceptor is in the form of a closed circuit, magnetic coupling between the susceptor and the electromagnet in use is enhanced, which results in greater or improved Joule heating.
- Magnetic hysteresis heating is a process in which an object made of a magnetic material is heated by penetrating the object with a varying magnetic field.
- a magnetic material can be considered to comprise many atomic-scale magnets, or magnetic dipoles. When a magnetic field penetrates such material, the magnetic dipoles align with the magnetic field. Therefore, when a varying magnetic field, such as an alternating magnetic field, for example as produced by an electromagnet, penetrates the magnetic material, the orientation of the magnetic dipoles changes with the varying applied magnetic field. Such magnetic dipole reorientation causes heat to be generated in the magnetic material.
- the filler may comprise one or more inorganic filler materials, such as calcium carbonate, perlite, vermiculite, diatomaceous earth, colloidal silica, magnesium oxide, magnesium sulphate, magnesium carbonate, and suitable inorganic sorbents, such as molecular sieves.
- the filler may comprise one or more organic filler materials such as wood pulp, cellulose and cellulose derivatives.
- the amorphous solid comprises no calcium carbonate such as chalk.
- the filler is fibrous.
- the filler may be a fibrous organic filler material such as wood pulp, hemp fibre, cellulose or cellulose derivatives.
- fibrous filler in an amorphous solid may increase the tensile strength of the material. This may be particularly advantageous in examples wherein the amorphous solid is provided as a sheet, such as when an amorphous solid sheet circumscribes a rod of aerosol-generating material.
- the amorphous solid does not comprise tobacco fibres. In particular embodiments, the amorphous solid does not comprise fibrous material.
- the aerosol generating material does not comprise tobacco fibres. In particular embodiments, the aerosol generating material does not comprise fibrous material.
- the aerosol-generating material does not comprise tobacco fibres. In particular embodiments, the aerosol-generating material does not comprise fibrous material.
- the aerosol-generating article does not comprise tobacco fibres. In particular embodiments, the aerosol-generating article does not comprise fibrous material.
- the amorphous solid may consist essentially of, or consist of a gelling agent, an aerosol generating agent, water, and menthol.
- the aerosol-generating material, or amorphous solid comprises one or more cannabinoid compounds selected from the group consisting of cannabidiol (CBD), tetrahydrocannabinol (THC), tetrahydrocannabinolic acid (THCA), cannabidiolic acid (CBDA), cannabinol (CBN), cannabigerol (CBG), cannabichromene (CBC), cannabicyclol (CBL), cannabivarin (CBV), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), cannabichromevarin (CBCV), cannabigerovarin (CBGV), cannabigerol monomethyl ether (CBGM) and cannabielsoin (CBE), cannabicitran (CBT).
- CBD cannabidiol
- THC tetrahydrocannabinol
- THCA tetrahydroc
- the aerosol-generating material may comprise one or more cannabinoid compounds selected from the group consisting of cannabidiol (CBD) and THC (tetrahydrocannabinol).
- CBD cannabidiol
- THC tetrahydrocannabinol
- the aerosol-generating material may comprise cannabidiol (CBD).
- CBD cannabidiol
- the aerosol-generating material may comprise nicotine and cannabidiol (CBD).
- CBD cannabidiol
- the aerosol-generating material may comprise nicotine, cannabidiol (CBD), and THC (tetrahydrocannabinol).
- the aerosol generating material comprising the amorphous solid may have any suitable area density, such as from 30 g/m 2 to 120 g/m 2 .
- aerosol generating material may have an area density of from about 30 to 70 g/m 2 , or about 40 to 60 g/m 2 .
- the amorphous solid may have an area density of from about 80 to 120 g/m 2 , or from about 70 to 110 g/m 2 , or particularly from about 90 to 110 g/m 2 .
- Such area densities may be particularly suitable where the aerosol-generating material is included in an aerosol-generating article/assembly in sheet form, or as a shredded sheet (described further hereinbelow).
- An aspect of the invention provides non-combustible aerosol provision system comprising an article according as described herein and non-combustible aerosol provision device comprising a heater which is configured to heat not burn the aerosol-generating article.
- a non-combustible aerosol provision system may also be referred to as an aerosol generating assembly.
- a non-combustible aerosol provision device may be referred to as an aerosol generating apparatus.
- the heater may heat, without burning, the aerosol-generating material to a temperature of less than 350 °C, such as between 120°C and 350 °C. In some cases, the heater may heat, without burning, the aerosol-generating material to between 140 °C and 250 °C in use, or between 220 °C and 280 °C. In some cases in use, substantially all of the amorphous solid is less than about 4mm, 3mm, 2mm or 1mm from the heater. In some cases, the solid is disposed between about 0.010mm and 2.0mm from the heater, suitably between about 0.02mm and 1.0mm, suitably 0.1mm to 0.5mm. These minimum distances may, in some cases, reflect the thickness of a support that supports the amorphous solid. In some cases, a surface of the amorphous solid may directly abut the heater.
- the heater is configured to heat not burn the aerosol-generating article, and thus the aerosol-generating material.
- the heater may be, in some cases, a thin film, electrically resistive heater. In other cases, the heater may comprise an induction heater or the like.
- the heater may be a combustible heat source or a chemical heat source which undergoes an exothermic reaction to product heat in use.
- the aerosol generating assembly may comprise a plurality of heaters. The heater(s) may be powered by a battery.
- the aerosol-generating article may additionally comprise a cooling element and/or a filter.
- the cooling element if present, may act or function to cool gaseous or aerosol components. In some cases, it may act to cool gaseous components such that they condense to form an aerosol. It may also act to space the very hot parts of the non-combustible aerosol provision device from the user.
- the filter if present, may comprise any suitable filter known in the art such as a cellulose acetate plug.
- the aerosol generating assembly may be a heat-not-burn device. That is, it may contain a solid tobacco-containing material (and no liquid aerosol-generating material). In some cases, the amorphous solid may comprise the tobacco material.
- a heat-not-burn device is disclosed in WO 2015/062983 A2 , which is incorporated by reference in its entirety.
- the aerosol generating assembly may be an electronic tobacco hybrid device. That is, it may contain a solid aerosol-generating material and a liquid aerosol-generating material.
- the amorphous solid may comprise nicotine.
- the amorphous solid may comprise a tobacco material.
- the amorphous solid may comprise a tobacco material and a separate nicotine source.
- the separate aerosol-generating materials may be heated by separate heaters, the same heater or, in one case, a downstream aerosol-generating material may be heated by a hot aerosol which is generated from the upstream aerosol-generating material.
- An electronic tobacco hybrid device is disclosed in WO 2016/135331 A1 , which is incorporated by reference in its entirety.
- the aerosol-generating material or amorphous solid may comprise an acid.
- the acid may be an organic acid.
- the acid may be at least one of a monoprotic acid, a diprotic acid and a triprotic acid.
- the acid may contain at least one carboxyl functional group.
- the acid may be at least one of an alpha-hydroxy acid, carboxylic acid, dicarboxylic acid, tricarboxylic acid and keto acid.
- the acid may be an alpha-keto acid.
- the acid may be at least one of succinic acid, lactic acid, benzoic acid, citric acid, tartaric acid, fumaric acid, levulinic acid, acetic acid, malic acid, formic acid, sorbic acid, benzoic acid, propanoic and pyruvic acid.
- the acid is lactic acid.
- the acid is benzoic acid.
- the acid may be an inorganic acid.
- the acid may be a mineral acid.
- the acid may be at least one of sulphuric acid, hydrochloric acid, boric acid and phosphoric acid.
- the acid is levulinic acid.
- an acid is particularly preferred in embodiments in which the aerosol-generating material or amorphous solid comprises nicotine.
- the presence of an acid may stabilise dissolved species in the slurry from which the aerosol-generating material or amorphous solid is formed.
- the presence of the acid may reduce or substantially prevent evaporation of nicotine during drying of the slurry, thereby reducing loss of nicotine during manufacturing.
- the amorphous solid may comprise a colourant.
- the addition of a colourant may alter the visual appearance of the amorphous solid.
- the presence of colourant in the amorphous solid may enhance the visual appearance of the amorphous solid and the aerosol-generating material.
- the amorphous solid may be colour-matched to other components of the aerosol-generating material or to other components of an article comprising the amorphous solid.
- colourants may be used depending on the desired colour of the amorphous solid.
- the colour of amorphous solid may be, for example, white, green, red, purple, blue, brown or black. Other colours are also envisaged.
- Natural or synthetic colourants such as natural or synthetic dyes, food-grade colourants and pharmaceutical-grade colourants may be used.
- the colourant is caramel, which may confer the amorphous solid with a brown appearance.
- the colour of the amorphous solid may be similar to the colour of other components (such as tobacco material) in an aerosol-generating material comprising the amorphous solid.
- the addition of a colourant to the amorphous solid renders it visually indistinguishable from other components in the aerosol-generating material.
- the colourant may be incorporated during the formation of the amorphous solid (e.g. when forming a slurry comprising the materials that form the amorphous solid) or it may be applied to the amorphous solid after its formation (e.g. by spraying it onto the amorphous solid).
- the aerosol-generating article (which may be referred to herein as an article, a cartridge or a consumable) may be adapted for use in a THP, an electronic tobacco hybrid device or another aerosol generating device.
- the article may additionally comprise a filter and/or cooling element (which have been described above).
- the aerosol-generating article may be circumscribed by a wrapping material such as paper.
- the aerosol-generating article may additionally comprise ventilation apertures. These may be provided in the sidewall of the article. In some cases, the ventilation apertures may be provided in the filter and/or cooling element. These apertures may allow cool air to be drawn into the article during use, which can mix with the heated volatilised components thereby cooling the aerosol.
- the ventilation enhances the generation of visible heated volatilised components from the article when it is heated in use.
- the heated volatilised components are made visible by the process of cooling the heated volatilised components such that supersaturation of the heated volatilised components occurs.
- the heated volatilised components then undergo droplet formation, otherwise known as nucleation, and eventually the size of the aerosol particles of the heated volatilised components increases by further condensation of the heated volatilised components and by coagulation of newly formed droplets from the heated volatilised components.
- the ratio of the cool air to the sum of the heated volatilised components and the cool air is at least 15%.
- a ventilation ratio of 15% enables the heated volatilised components to be made visible by the method described above. The visibility of the heated volatilised components enables the user to identify that the volatilised components have been generated and adds to the sensory experience of the smoking experience.
- the ventilation ratio is between 50% and 85% to provide additional cooling to the heated volatilised components. In some cases, the ventilation ratio may be at least 60% or 65%.
- the aerosol generating material may be included in the article/assembly in sheet form. In some cases, the aerosol generating material may be included as a planar sheet. In some cases, the aerosol generating material may be included as a planar sheet, as a bunched or gathered sheet, as a crimped sheet, or as a rolled sheet (i.e. in the form of a tube). In some such cases, the amorphous solid of these embodiments may be included in an aerosol-generating article/assembly as a sheet, such as a sheet circumscribing a rod of aerosol-generating material (e.g. tobacco). In some other cases, the aerosol generating material may be formed as a sheet and then shredded and incorporated into the article. In some cases, the shredded sheet may be mixed with cut rag tobacco and incorporated into the article.
- the aerosol generating material may be formed as a sheet and then shredded and incorporated into the article. In some cases, the shredded sheet may be mixed with cut
- the amorphous solid in sheet form may have a tensile strength of from around 200 N/m to around 900 N/m. In some examples, such as where the amorphous solid does not comprise a filler, the amorphous solid may have a tensile strength of from 200 N/m to 400 N/m, or 200 N/m to 300 N/m, or about 250 N/m. Such tensile strengths may be particularly suitable for embodiments wherein the aerosol generating material is formed as a sheet and then shredded and incorporated into an aerosol-generating article.
- the amorphous solid may have a tensile strength of from 600 N/m to 900 N/m, or from 700 N/m to 900 N/m, or around 800 N/m.
- tensile strengths may be particularly suitable for embodiments wherein the aerosol generating material is included in an aerosol-generating article/assembly as a rolled sheet, suitably in the form of a tube.
- the assembly may comprise an integrated aerosol-generating article and heater, or may comprise a heater device into which the article is inserted in use.
- FIG. 1 and 2 there are shown a partially cut-away section view and a perspective view of an example of an aerosol-generating article 101.
- the article 101 is adapted for use with a device having a power source and a heater.
- the article 101 of this embodiment is particularly suitable for use with the device 51 shown in Figures 5 to 7 , described below.
- the article 101 may be removably inserted into the device shown in Figure 5 at an insertion point 20 of the device 51.
- the article 101 of one example is in the form of a substantially cylindrical rod that includes a body of aerosol generating material 103 and a filter assembly 105 in the form of a rod.
- the aerosol generating material comprises the amorphous solid material described herein. In some embodiments, it may be included in sheet form. In some embodiments it may be included in the form of a shredded sheet. In some embodiments, the aerosol generating material described herein may be incorporated in sheet form and in shredded form.
- the filter assembly 105 includes three segments, a cooling segment 107, a filter segment 109 and a mouth end segment 111.
- the article 101 has a first end 113, also known as a mouth end or a proximal end and a second end 115, also known as a distal end.
- the body of aerosol generating material 103 is located towards the distal end 115 of the article 101.
- the cooling segment 107 is located adjacent the body of aerosol generating material 103 between the body of aerosol generating material 103 and the filter segment 109, such that the cooling segment 107 is in an abutting relationship with the aerosol generating material 103 and the filter segment 103.
- the filter segment 109 is located in between the cooling segment 107 and the mouth end segment 111.
- the mouth end segment 111 is located towards the proximal end 113 of the article 101, adjacent the filter segment 109.
- the filter segment 109 is in an abutting relationship with the mouth end segment 111.
- the total length of the filter assembly 105 is between 37mm and 45mm, more preferably, the total length of the filter assembly 105 is 41mm.
- the rod of aerosol generating material 103 is between 34mm and 50mm in length, suitably between 38mm and 46mm in length, suitably 42mm in length.
- the total length of the article 101 is between 71mm and 95mm, suitably between 79mm and 87mm, suitably 83mm.
- an axial end of the body of aerosol generating material 103 is visible at the distal end 115 of the article 101.
- the distal end 115 of the article 101 may comprise an end member (not shown) covering the axial end of the body of aerosol generating material 103.
- the body of aerosol generating material 103 is joined to the filter assembly 105 by annular tipping paper (not shown), which is located substantially around the circumference of the filter assembly 105 to surround the filter assembly 105 and extends partially along the length of the body of aerosol generating material 103.
- the tipping paper is made of 58GSM standard tipping base paper.
- the tipping paper has a length of between 42mm and 50mm, suitably of 46mm.
- the cooling segment 107 is an annular tube and is located around and defines an air gap within the cooling segment.
- the air gap provides a chamber for heated volatilised components generated from the body of aerosol generating material 103 to flow.
- the cooling segment 107 is hollow to provide a chamber for aerosol accumulation yet rigid enough to withstand axial compressive forces and bending moments that might arise during manufacture and whilst the article 101 is in use during insertion into the device 51.
- the thickness of the wall of the cooling segment 107 is approximately 0.29mm.
- the cooling segment 107 provides a physical displacement between the aerosol generating material 103 and the filter segment 109.
- the physical displacement provided by the cooling segment 107 will provide a thermal gradient across the length of the cooling segment 107.
- the cooling segment 107 is configured to provide a temperature differential of at least 40 degrees Celsius between a heated volatilised component entering a first end of the cooling segment 107 and a heated volatilised component exiting a second end of the cooling segment 107.
- the cooling segment 107 is configured to provide a temperature differential of at least 60 degrees Celsius between a heated volatilised component entering a first end of the cooling segment 107 and a heated volatilised component exiting a second end of the cooling segment 107.
- This temperature differential across the length of the cooling element 107 protects the temperature sensitive filter segment 109 from the high temperatures of the aerosol generating material 103 when it is heated by the device 51. If the physical displacement was not provided between the filter segment 109 and the body of aerosol generating material 103 and the heating elements of the device 51, then the temperature sensitive filter segment may 109 become damaged in use, so it would not perform its required functions as effectively.
- the length of the cooling segment 107 is at least 15mm. In one example, the length of the cooling segment 107 is between 20mm and 30mm, more particularly 23mm to 27mm, more particularly 25mm to 27mm, suitably 25mm.
- the cooling segment 107 is made of paper, which means that it is comprised of a material that does not generate compounds of concern, for example, toxic compounds when in use adjacent to the heater of the device 51.
- the cooling segment 107 is manufactured from a spirally wound paper tube which provides a hollow internal chamber yet maintains mechanical rigidity. Spirally wound paper tubes are able to meet the tight dimensional accuracy requirements of high-speed manufacturing processes with respect to tube length, outer diameter, roundness and straightness.
- the cooling segment 107 is a recess created from stiff plug wrap or tipping paper.
- the stiff plug wrap or tipping paper is manufactured to have a rigidity that is sufficient to withstand the axial compressive forces and bending moments that might arise during manufacture and whilst the article 101 is in use during insertion into the device 51.
- the filter segment 109 may be formed of any filter material sufficient to remove one or more volatilised compounds from heated volatilised components from the aerosol generating material.
- the filter segment 109 is made of a mono-acetate material, such as cellulose acetate.
- the filter segment 109 provides cooling and irritation-reduction from the heated volatilised components without depleting the quantity of the heated volatilised components to an unsatisfactory level for a user.
- a capsule (not illustrated) may be provided in filter segment 109. It may be disposed substantially centrally in the filter segment 109, both across the filter segment 109 diameter and along the filter segment 109 length. In other cases, it may be offset in one or more dimension.
- the capsule may in some cases, where present, contain a volatile component such as a flavourant or aerosol generating agent.
- the density of the cellulose acetate tow material of the filter segment 109 controls the pressure drop across the filter segment 109, which in turn controls the draw resistance of the article 101. Therefore the selection of the material of the filter segment 109 is important in controlling the resistance to draw of the article 101. In addition, the filter segment performs a filtration function in the article 101.
- the filter segment 109 is made of a 8Y15 grade of filter tow material, which provides a filtration effect on the heated volatilised material, whilst also reducing the size of condensed aerosol droplets which result from the heated volatilised material.
- the presence of the filter segment 109 provides an insulating effect by providing further cooling to the heated volatilised components that exit the cooling segment 107. This further cooling effect reduces the contact temperature of the user's lips on the surface of the filter segment 109.
- the filter segment 109 is between 6mm to 10mm in length, suitably 8mm.
- the mouth end segment 111 is an annular tube and is located around and defines an air gap within the mouth end segment 111.
- the air gap provides a chamber for heated volatilised components that flow from the filter segment 109.
- the mouth end segment 111 is hollow to provide a chamber for aerosol accumulation yet rigid enough to withstand axial compressive forces and bending moments that might arise during manufacture and whilst the article is in use during insertion into the device 51.
- the thickness of the wall of the mouth end segment 111 is approximately 0.29mm.
- the length of the mouth end segment 111 is between 6mm to 10mm, suitably 8mm.
- the mouth end segment 111 may be manufactured from a spirally wound paper tube which provides a hollow internal chamber yet maintains critical mechanical rigidity. Spirally wound paper tubes are able to meet the tight dimensional accuracy requirements of high-speed manufacturing processes with respect to tube length, outer diameter, roundness and straightness.
- the mouth end segment 111 provides the function of preventing any liquid condensate that accumulates at the exit of the filter segment 109 from coming into direct contact with a user.
- the mouth end segment 111 and the cooling segment 107 may be formed of a single tube and the filter segment 109 is located within that tube separating the mouth end segment 111 and the cooling segment 107.
- FIGS 3 and 4 there are shown a partially cut-away section and perspective views of an example of an article 301.
- the reference signs shown in Figures 3 and 4 are equivalent to the reference signs shown in Figures 1 and 2 , but with an increment of 200.
- a ventilation region 317 is provided in the article 301 to enable air to flow into the interior of the article 301 from the exterior of the article 301.
- the ventilation region 317 takes the form of one or more ventilation holes 317 formed through the outer layer of the article 301.
- the ventilation holes may be located in the cooling segment 307 to aid with the cooling of the article 301.
- the ventilation region 317 comprises one or more rows of holes, and preferably, each row of holes is arranged circumferentially around the article 301 in a cross-section that is substantially perpendicular to a longitudinal axis of the article 301.
- each row of ventilation holes may have between 12 to 36 ventilation holes 317.
- the ventilation holes 317 may, for example, be between 100 to 500 ⁇ m in diameter.
- an axial separation between rows of ventilation holes 317 is between 0.25mm and 0.75mm, suitably 0.5mm.
- the ventilation holes 317 are of uniform size. In another example, the ventilation holes 317 vary in size.
- the ventilation holes can be made using any suitable technique, for example, one or more of the following techniques: laser technology, mechanical perforation of the cooling segment 307 or pre-perforation of the cooling segment 307 before it is formed into the article 301.
- the ventilation holes 317 are positioned so as to provide effective cooling to the article 301.
- the rows of ventilation holes 317 are located at least 11mm from the proximal end 313 of the article, suitably between 17mm and 20mm from the proximal end 313 of the article 301.
- the location of the ventilation holes 317 is positioned such that user does not block the ventilation holes 317 when the article 301 is in use.
- Providing the rows of ventilation holes between 17mm and 20mm from the proximal end 313 of the article 301 enables the ventilation holes 317 to be located outside of the device 51, when the article 301 is fully inserted in the device 51, as can be seen in Figures 6 and 7 .
- By locating the ventilation holes outside of the device non-heated air is able to enter the article 301 through the ventilation holes from outside the device 51 to aid with the cooling of the article 301.
- the length of the cooling segment 307 is such that the cooling segment 307 will be partially inserted into the device 51, when the article 301 is fully inserted into the device 51.
- the length of the cooling segment 307 provides a first function of providing a physical gap between the heater arrangement of the device 51 and the heat sensitive filter arrangement 309, and a second function of enabling the ventilation holes 317 to be located in the cooling segment, whilst also being located outside of the device 51, when the article 301 is fully inserted into the device 51.
- the majority of the cooling element 307 is located within the device 51. However, there is a portion of the cooling element 307 that extends out of the device 51. It is in this portion of the cooling element 307 that extends out of the device 51 in which the ventilation holes 317 are located.
- FIG. 5 to 7 there is shown an example of a device 51 arranged to heat aerosol generating material to volatilise at least one component of said aerosol generating material, typically to form an aerosol which can be inhaled.
- the device 51 is a heating device which releases compounds by heating, but not burning, the aerosol generating material.
- a first end 53 is sometimes referred to herein as the mouth or proximal end 53 of the device 51 and a second end 55 is sometimes referred to herein as the distal end 55 of the device 51.
- the device 51 has an on/off button 57 to allow the device 51 as a whole to be switched on and off as desired by a user.
- the device 51 comprises a housing 59 for locating and protecting various internal components of the device 51.
- the housing 59 comprises a uni-body sleeve 11 that encompasses the perimeter of the device 51, capped with a top panel 17 which defines generally the 'top' of the device 51 and a bottom panel 19 which defines generally the 'bottom' of the device 51.
- the housing comprises a front panel, a rear panel and a pair of opposite side panels in addition to the top panel 17 and the bottom panel 19.
- the top panel 17 and/or the bottom panel 19 may be removably fixed to the uni-body sleeve 11, to permit easy access to the interior of the device 51, or may be "permanently" fixed to the uni-body sleeve 11, for example to deter a user from accessing the interior of the device 51.
- the panels 17 and 19 are made of a plastics material, including for example glass-filled nylon formed by injection moulding, and the uni-body sleeve 11 is made of aluminium, though other materials and other manufacturing processes may be used.
- the top panel 17 of the device 51 has an opening 20 at the mouth end 53 of the device 51 through which, in use, the article 101, 301 including the aerosol generating material may be inserted into the device 51 and removed from the device 51 by a user.
- the housing 59 has located or fixed therein a heater arrangement 23, control circuitry 25 and a power source 27.
- the heater arrangement 23, the control circuitry 25 and the power source 27 are laterally adjacent (that is, adjacent when viewed from an end), with the control circuitry 25 being located generally between the heater arrangement 23 and the power source 27, though other locations are possible.
- the control circuitry 25 may include a controller, such as a microprocessor arrangement, configured and arranged to control the heating of the aerosol generating material in the article 101, 301 as discussed further below.
- a controller such as a microprocessor arrangement
- the power source 27 may be for example a battery, which may be a rechargeable battery or a non-rechargeable battery.
- suitable batteries include for example a lithium-ion battery, a nickel battery (such as a nickel-cadmium battery), an alkaline battery and/ or the like.
- the battery 27 is electrically coupled to the heater arrangement 23 to supply electrical power when required and under control of the control circuitry 25 to heat the aerosol generating material in the article (as discussed, to volatilise the aerosol generating material without causing the aerosol generating material to burn).
- An advantage of locating the power source 27 laterally adjacent to the heater arrangement 23 is that a physically large power source 25 may be used without causing the device 51 as a whole to be unduly lengthy.
- a physically large power source 25 has a higher capacity (that is, the total electrical energy that can be supplied, often measured in Amp-hours or the like) and thus the battery life for the device 51 can be longer.
- the heater arrangement 23 is generally in the form of a hollow cylindrical tube, having a hollow interior heating chamber 29 into which the article 101, 301 comprising the aerosol generating material is inserted for heating in use.
- the heater arrangement 23 may comprise a single heating element or may be formed of plural heating elements aligned along the longitudinal axis of the heater arrangement 23.
- the or each heating element may be annular or tubular, or at least part-annular or part-tubular around its circumference.
- the or each heating element may be a thin film heater.
- the or each heating element may be made of a ceramics material.
- suitable ceramics materials include alumina and aluminium nitride and silicon nitride ceramics, which may be laminated and sintered.
- Other heating arrangements are possible, including for example inductive heating, infrared heater elements, which heat by emitting infrared radiation, or resistive heating elements formed by for example a resistive electrical winding.
- the heater arrangement 23 is supported by a stainless steel support tube and comprises a polyimide heating element.
- the heater arrangement 23 is dimensioned so that substantially the whole of the body of aerosol generating material 103, 303 of the article 101, 301 is inserted into the heater arrangement 23 when the article 101, 301 is inserted into the device 51.
- the or each heating element may be arranged so that selected zones of the aerosol generating material can be independently heated, for example in turn (over time, as discussed above) or together (simultaneously) as desired.
- the heater arrangement 23 in this example is surrounded along at least part of its length by a thermal insulator 31.
- the insulator 31 helps to reduce heat passing from the heater arrangement 23 to the exterior of the device 51. This helps to keep down the power requirements for the heater arrangement 23 as it reduces heat losses generally.
- the insulator 31 also helps to keep the exterior of the device 51 cool during operation of the heater arrangement 23.
- the insulator 31 may be a double-walled sleeve which provides a low pressure region between the two walls of the sleeve. That is, the insulator 31 may be for example a "vacuum" tube, i.e. a tube that has been at least partially evacuated so as to minimise heat transfer by conduction and/or convection.
- Other arrangements for the insulator 31 are possible, including using heat insulating materials, including for example a suitable foam-type material, in addition to or instead of a double-walled sleeve.
- the housing 59 may further comprises various internal support structures 37 for supporting all internal components, as well as the heating arrangement 23.
- the device 51 further comprises a collar 33 which extends around and projects from the opening 20 into the interior of the housing 59 and a generally tubular chamber 35 which is located between the collar 33 and one end of the vacuum sleeve 31.
- the chamber 35 further comprises a cooling structure 35f, which in this example, comprises a plurality of cooling fins 35f spaced apart along the outer surface of the chamber 35, and each arranged circumferentially around outer surface of the chamber 35.
- the air gap 36 is around all of the circumference of the article 101, 301 over at least part of the cooling segment 307.
- the collar 33 comprises a plurality of ridges 60 arranged circumferentially around the periphery of the opening 20 and which project into the opening 20.
- the ridges 60 take up space within the opening 20 such that the open span of the opening 20 at the locations of the ridges 60 is less than the open span of the opening 20 at the locations without the ridges 60.
- the ridges 60 are configured to engage with an article 101, 301 inserted into the device to assist in securing it within the device 51.
- Open spaces (not shown in the Figures) defined by adjacent pairs of ridges 60 and the article 101, 301 form ventilation paths around the exterior of the article 101, 301. These ventilation paths allow hot vapours that have escaped from the article 101, 301 to exit the device 51 and allow cooling air to flow into the device 51 around the article 101, 301 in the air gap 36.
- the article 101, 301 is removably inserted into an insertion point 20 of the device 51, as shown in Figures 5 to 7 .
- the body of aerosol generating material 103, 303 which is located towards the distal end 115, 315 of the article 101, 301, is entirely received within the heater arrangement 23 of the device 51.
- the proximal end 113, 313 of the article 101, 301 extends from the device 51 and acts as a mouthpiece assembly for a user.
- the heater arrangement 23 will heat the article 101, 301 to volatilise at least one component of the aerosol generating material from the body of aerosol generating material 103, 303.
- the primary flow path for the heated volatilised components from the body of aerosol generating material 103, 303 is axially through the article 101, 301, through the chamber inside the cooling segment 107, 307, through the filter segment 109, 309, through the mouth end segment 111, 313 to the user.
- the temperature of the heated volatilised components that are generated from the body of aerosol generating material is between 60°C and 250°C, which may be above the acceptable inhalation temperature for a user.
- the heated volatilised component travels through the cooling segment 107, 307, it will cool and some volatilised components will condense on the inner surface of the cooling segment 107, 307.
- cool air will be able to enter the cooling segment 307 via the ventilation holes 317 formed in the cooling segment 307. This cool air will mix with the heated volatilised components to provide additional cooling to the heated volatilised components.
- Another aspect of the invention provides a method of making an aerosol-generating material according to the first aspect, the method comprising (a) providing slurry comprising the gelling agent, aerosol-former material and menthol, (b) forming a layer of the slurry, (c) setting the slurry to form a gel, and (d) drying to form an amorphous solid.
- the (b) forming a layer the of the slurry may comprise spraying, casting or extruding the slurry, for example.
- the slurry layer is formed by electrospraying the slurry.
- the slurry layer is formed by casting the slurry.
- the (b) and/or (c) and/or (d) may, at least partially, occur simultaneously (for example, during electrospraying). In some cases, (b), (c) and (d) may occur sequentially.
- the slurry is applied to a support.
- the layer may be formed on a support.
- the slurry comprises gelling agent, aerosol-former material and menthol.
- the slurry may comprise these components in any of the proportions given herein in relation to the composition of the aerosol-generating material.
- the slurry may comprise:
- the slurry may comprise a gelling agent precursor.
- the slurry may comprise sodium, potassium or ammonium alginate as a gel-precursor.
- G units and M units are present in the gelling agent precursor in a molar ratio of from 1:2 to 10:1 (i.e. the number of ⁇ -(1-4)-linked L-guluronate units present compared with the number of ⁇ -(1-4)-linked D-mannuronate units).
- the G units and M units are present in a molar ratio of from 1:3 to 3:1, or from 1:2 to 2:1, or from 1:1.5 to 1.5:1, or from 1:1.2 to 1.2:1.
- the setting the gel (c) may comprise the addition of a setting agent to the slurry.
- (c) may comprise the addition of Ca 2+ cations to the slurry.
- the Ca 2+ cations may be provided as part of a calcium source.
- the slurry may comprise sodium, potassium or ammonium alginate as a gel-precursor, and a setting agent comprising a calcium source (such as a calcium salt, e.g. calcium chloride), may be added to the slurry to form a calcium-crosslinked alginate gel.
- the Ca 2+ calcium source is supplied to the slurry in an amount such that the molar ratio of Ca 2+ cations to G units in the slurry is from 0.2:1 to 1:1, or from 0.3:1 to 0.5:1 or approximately 0.4:1 ("approximately" allowing for a 20% tolerance).
- the setting agent, or the calcium source comprises or consists of calcium acetate, calcium formate, calcium carbonate, calcium hydrogencarbonate, calcium chloride, calcium lactate, or a combination thereof.
- the setting agent, or the calcium source comprises or consists of calcium formate and/or calcium lactate.
- the setting agent, or the calcium source comprises or consists of calcium formate. The inventors have identified that, typically, employing calcium formate as a setting agent, or the calcium source, results in an amorphous solid having a greater tensile strength and greater resistance to elongation.
- Ca 2+ cations are provided to the slurry as part of a fluid system comprising a calcium source and an aqueous carrier.
- the calcium source may comprise a combination of calcium-containing compounds.
- the calcium source comprises one or more calcium salts such as calcium chloride, calcium lactate, calcium citrate, calcium acetate, or calcium citrate.
- the calcium source is dissolved and optionally suspended in the aqueous carrier. In some examples, the calcium source is present in the fluid system in an amount which is greater than is soluble in the aqueous carrier under normal temperature and pressure.
- the normal temperature and pressure is as defined by the National Institute of Standards and Technology, and refers to a temperature of 20 °C and an absolute pressure of 1 atm.
- the fluid source is a supersaturated solution of calcium source, such as a supersaturated solution of calcium salt(s).
- the fluid source comprises dissolved and suspended (particulate) calcium source, such as dissolved and suspended (particulate) calcium salt.
- the drying (d) may, in some cases, remove from about 50wt%, 60wt%, 70wt%, 80wt% or 90wt% to about 80wt%, 90wt% or 95wt% (WWB) of water in the slurry.
- the drying (d) may, in some cases, may reduce the cast material thickness by at least 80%, suitably 85% or 87%.
- the slurry may be cast at a thickness of 2mm, and the resulting dried amorphous solid material may have a thickness of 0.2mm.
- the slurry itself may also form part of the invention.
- the slurry solvent may consist essentially of or consist of water.
- the slurry may comprise from about 50wt%, 60wt%, 70wt%, 80wt% or 90wt% of solvent (WWB).
- the slurry has a viscosity of from about 10 to about 20 Pa ⁇ s at 46.5 °C, such as from about 14 to about 16 Pa ⁇ s at 46.5 °C.
- the dry weight content of the slurry may match the dry weight content of the amorphous solid.
- the discussion herein relating to the solid composition is explicitly disclosed in combination with the slurry aspect of the invention.
- the method comprises heating the aerosol-generating material to a temperature of less than 350 °C. In some embodiments, the method comprises heating the aerosol-generating material to a temperature of from about 220 °C to about 280 °C. In some embodiments, the method comprises heating at least a portion of the aerosol-generating material to a temperature of from about 220 °C to about 280 °C over a session of use.
- Session of use refers to a single period of use of the non-combustible aerosol provision system by a user.
- the session of use begins at the point at which power is first supplied to at least one heating unit present in the heating assembly.
- the device will be ready for use after a period of time has elapsed from the start of the session of use.
- the session of use ends at the point at which no power is supplied to any of the heating elements in the aerosol-generating device.
- the end of the session of use may coincide with the point at which the smoking article is depleted (the point at which the total particulate matter yield (mg) in each puff would be deemed unacceptably low by a user).
- the session will have a duration of a plurality of puffs.
- Said session may have a duration less than 7 minutes, or 6 minutes, or 5 minutes, or 4 minutes and 30 seconds, or 4 minutes, or 3 minutes and 30 seconds.
- the session of use may have a duration of from 2 to 5 minutes, or from 3 to 4.5 minutes, or 3.5 to 4.5 minutes, or suitably 4 minutes.
- a session may be initiated by the user actuating a button or switch on the device, causing at least one heating element to begin rising in temperature.
- At least 20wt% of the menthol present in the amorphous solid is aerosolised, or at least 30wt%, 40wt% or 50wt%. That is, after a session of use, the amount of menthol in the amorphous solid is depleted by 20wt%, 30wt%, 40wt% or 50wt%.
- the molar ratio of Ca 2+ to G units in the amorphous solid as described herein my allow for efficient delivery of menthol to a user (e.g. a high proportion of active material is aerosolised from the amorphous solid) whilst maintaining a long shelf-life before the amorphous solid is heated by the non-combustible aerosol provision device.
- a first aerosol-generating material and a second aerosol-generating material were prepared according to methods described herein. Both aerosol-generating materials were prepared from slurries having the following composition (w/w dry weight basis):
- the aerosol-generating materials differed only in the amount of calcium lactate which was supplied to the slurry to cross-link the alginate.
- the first aerosol-generating material was prepared by supplying calcium lactate to the slurry in an amount such that the molar ratio of Ca 2+ cations to G units in the sodium alginate was 0.4:1; the second aerosol-generating material was prepared by supplying calcium lactate to the slurry in an amount such that the molar ratio of Ca 2+ cations to G units in the sodium alginate was 0.2:1.
- the dried material was formed as a sheet, which was subsequently shredded and combined with tobacco to provide a blend.
- Each blend of aerosol-generating material and tobacco was formed into a rod consumable and provided with a filter as described herein, providing a first consumable comprising the first aerosol-generating material and a second consumable comprising the second aerosol-generating material.
- the puff-by-puff analysis was carried out according to the Health Canada Intense (HCI) puffing regime: no vent blocking, 55mL puff over two seconds, every 30 seconds.
- HCI Health Canada Intense
- Each puff was captured in a gas-tight syringe attached to a smoke engine.
- the captured sample was extracted with solvent and analysed with Gas Chromatography with Flame-Ionization Detection (GC-FID) for quantification of menthol against a calibration range.
- GC-FID Gas Chromatography with Flame-Ionization Detection
- Figure 8 depicts the results of this analysis. As can be seen, both materials give acceptable puff-by-puff menthol sensory performance.
- the first material having a molar ratio of Ca 2+ cations to G units of 0.4:1, was in particular found to provide desirable puff-by-puff menthol sensory performance.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Botany (AREA)
- Agronomy & Crop Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Preparation (AREA)
- Manufacture Of Tobacco Products (AREA)
- Cosmetics (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Containers And Packaging Bodies Having A Special Means To Remove Contents (AREA)
Description
- The present invention relates to aerosol generation.
- Smoking articles such as cigarettes, cigars and the like burn tobacco during use to create tobacco smoke. Alternatives to these types of articles release an inhalable aerosol or vapour by releasing compounds from a substrate material by heating without burning. These may be referred to as non-combustible smoking articles or aerosol generating assemblies.
- One example of such a product is a heating device which release compounds by heating, but not burning, a solid aerosol-generating material. This solid aerosol-generating material may, in some cases, contain a tobacco material. The heating volatilises at least one component of the material, typically forming an inhalable aerosol. These products may be referred to as heat-not-burn devices, tobacco heating devices or tobacco heating products. Various different arrangements for volatilising at least one component of the solid aerosol-generating material are known.
- As another example, there are e-cigarette / tobacco heating product hybrid devices, also known as electronic tobacco hybrid devices. These hybrid devices contain a liquid source (which may or may not contain nicotine) which is vaporised by heating to produce an inhalable vapour or aerosol. The device additionally contains a solid aerosol-generating material (which may or may not contain a tobacco material) and components of this material are entrained in the inhalable vapour or aerosol to produce the inhaled medium.
-
US 2011/104218 describes capsules for smoking articles prepared by forming hydrogel capsules of specific diameter with at least one coating layer. -
WO 2014/083333 describes a smokable material having a controlled filling value. -
WO 2011/117748 describes a method for providing an encapsulated flavourant and/or chemesthetic agent in a smoking article. -
WO 2016/184977 describes a solid aerosol generating material that comprises about 5-35 wt% tobacco extract, about 50-80 wt% filler, about 10-35 wt% aerosol generating agent and about 2.5-10 wt% binder. -
WO 2005/058078 describes a smoking article comprising discrete segments of smokable material having an encapsulated flavourant contained within a component of the smokable material. - According to a first aspect of the present invention, there is provided an aerosol-generating material comprising an amorphous solid, the amorphous solid comprising:
- 0.1-80 wt% of menthol;
- 1-60 wt% of a gelling agent, the gelling agent comprising calcium-crosslinked alginate which comprises α-(1-4)-linked L-guluronate (G) units; and
- 0.1-50 wt% of an aerosol-former material.
- According to a second third aspect of the present invention, there is provided a substrate comprising an aerosol-generating material as described herein and a support on which the aerosol-generating material is provided.
- According to a further aspect of the present invention, there is provided an article for use with a non-combustible aerosol provision device, the article comprising an aerosol-generating material as described herein and/or a substrate as described herein. According to a further aspect of the present invention, there is provided a non-combustible aerosol provision system comprising an article as described herein and a non-combustible aerosol provision device, wherein the non-combustible aerosol provision device is configured to generate aerosol from the article when the article is used with the non-combustible aerosol provision device, wherein the non-combustible aerosol provision device comprises a heater configured to heat but not burn the article.
- According to a further aspect of the present invention, there is provided a method of making an aerosol-generating material as described herein.
- According to a further aspect of the present invention, there is provided a method of generating an aerosol using a non-combustible aerosol provision system as described herein, the method comprising heating the aerosol-generating material. In some embodiments, the method comprises heating the aerosol-generating material to a temperature of less than 350 °C. In some embodiments, the method comprises heating the aerosol-generating material to a temperature of from about 220 °C to about 280 °C.
- Further features and advantages of the invention will become apparent from the following description of preferred embodiments of the invention, given by way of example only, which is made with reference to the accompanying drawings.
-
-
Figure 1 shows a section view of an example of an aerosol-generating article. -
Figure 2 shows a perspective view of the article ofFigure 1 . -
Figure 3 shows a sectional elevation of an example of an aerosol-generating article. -
Figure 4 shows a perspective view of the article ofFigure 3 . -
Figure 5 shows a perspective view of an example of an aerosol generating assembly. -
Figure 6 shows a section view of an example of an aerosol generating assembly. -
Figure 7 shows a perspective view of an example of an aerosol generating assembly. -
Figure 8 shows puff-by-puff sensory data for examples of aerosol-generating materials. - The aerosol-generating material described herein is material that is capable of generating aerosol, for example when heated, irradiated or energized in any other way. Aerosol-generating material may, for example, be in the form of a solid, liquid or gel which may or may not contain nicotine and/or flavourants. The aerosol-generating material comprises an "amorphous solid", which may alternatively be referred to as a "monolithic solid" (i.e. non-fibrous). In some embodiments, the amorphous solid may be a dried gel. The amorphous solid is a solid material that may retain some fluid, such as liquid, within it. In some embodiments, the aerosol-generating material may for example comprise from about 50wt%, 60wt% or 70wt% of amorphous solid, to about 90wt%, 95wt% or 100wt% of amorphous solid. In some cases, the aerosol generating material consists of amorphous solid.
- As described hereinabove, the invention provides aerosol-generating material comprising an amorphous solid, the amorphous solid comprising:
- 0.1-80 wt% of menthol;
- 1-60 wt% of a gelling agent, the gelling agent comprising calcium-crosslinked alginate which comprises α-(1-4)-linked L-guluronate (G) units; and
- 0.1-50 wt% of an aerosol-former material.
- The gelling agent of the present invention comprises alginate salts (also referred to as "alginate"). Alginate salts are derivatives of alginic acid, and are linear polysaccharides comprising G units and typically M units. On addition of divalent cations to alginic acid, the alginate crosslinks to form a gel.
- As used herein, "G unit" refers to α-(1-4)-linked L-guluronate. α-L-guluronate is the conjugate base of α-L-guluronic acid. A G unit may also be referred to as a guluronate momomer, or a G residue. As used herein, "M unit" refers to β-(1-4)-linked D-mannuronate. β-D-mannuronate is the conjugate base of β-D-mannuronic acid. An M unit may also be referred to as a mannuronate monomer, or an M residue.
- Divalent cations such as Ca2+ interact with the carboxylate groups of the alginate monomers to form ionic crosslinks; the amorphous solid of the present invention comprises calcium-crosslinked alginate. The inventors have established that the physical characteristics of an amorphous solid comprising calcium-crosslinked alginate depends on the molar ratio of calcium cations (Ca2+) to, in particular, the alginate G units in the amorphous solid.
- The amorphous solid of the present invention comprises menthol. Menthol is present in the amorphous solid as an active substance. That is, menthol is included in the amorphous solid such that, upon heating of the amorphous solid, menthol is aerosolised and may be delivered to a user in order to achieve a physiological and/or olfactory response.
- Due to the physical characteristics of menthol (e.g. its volatility, solubility and so on), it is difficult to provide a menthol-containing amorphous solid which has an acceptable shelf-life and delivers an acceptable inhalable aerosol to a user when heated in a non-combustible aerosol provision system. On the one hand, the amorphous solid should retain a desirable amount of menthol during storage until the point at which the amorphous solid heated in a non-combustible aerosol provision system. On the other hand, the amorphous solid should be configured to release a desirable amount of menthol as part of an inhalable aerosol upon heating of the amorphous solid.
- The present inventors have identified that configuring the amorphous solid such that the molar ratio of Ca2+ to G units in the alginate is from 0.2 to 1 provides a menthol-containing aerosol-generating material which has a good shelf-life and also releases a desirable amount of menthol upon heating of the aerosol-generating material in a non-combustible aerosol provision device. In some embodiments, the molar ratio of Ca2+ to G units in the alginate is from 0.3:1 to 0.5:1. In some embodiments, the molar ratio of Ca2+ to G units in the alginate is approximately 0.4:1 ("approximately" allowing for a 20% tolerance).
- Without wishing to be bound by theory, it is believed that an amorphous solid having a Ca2+ content higher than that of the present invention would result in syneresis and thus deterioration of the aerosol-generating material during storage, and an amorphous solid having a Ca2+ content lower than that of the present invention would not retain a desirable amount of menthol after storage.
- In examples, the calcium-crosslinked alginate comprises a combination of G units and M units. In some embodiments, the G units and M units are present in a molar ratio of from 1:2 to 10:1 (i.e. the number of α-(1-4)-linked L-guluronate units present compared with the number of (β-(1-4)-linked D-mannuronate units). In some embodiments, the G units and M units are present in a molar ratio of from 1:3 to 3:1, or from 1:2 to 2:1, or from 1:1.5 to 1.5:1, or from 1:1.2 to 1.2:1.
- In some embodiments, when stored for 30 days in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), the aerosol-generating material contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- In some embodiments, when stored for 6 weeks (42 days) in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), the aerosol-generating material contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- In some embodiments, when stored for 16 weeks (112 days) in a sealed container under ambient conditions in accordance with ISO 3402 (22 °C; 60% relative humidity; 1013 mbar), the aerosol-generating material contains at least 60%, 70%, 80%, or 90% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- In some embodiments, alginate is comprised in the gelling agent in an amount of from 15-40wt% of the amorphous solid. That is, the amorphous solid comprises alginate in an amount of 15-40wt% by dry weight of the amorphous solid. In some embodiments, the amorphous solid comprises alginate in an amount of from 10-35wt%, or 15wt% to 30wt%.
- In some embodiments, the gelling agent further comprises pectin. In some embodiments, the alginate and pectin are present in a ratio of alginate to pectin of from 1:1 to 10:1. In some embodiments, the ratio of alginate to pectin is from 3:1 to 8:1, or 5:1 to 7: 1.The ratio of alginate to pectin is expressed as a dry weight ratio (w/w).
- The inventors have established that providing a gelling agent comprising alginate and pectin in such ratios may provide an improved amorphous solid. Without wishing to be bound by theory, it is believed that a combination of alginate and pectin may have a synergistic effect on the binding in the amorphous solid. Further, combining alginate and pectin in particular ratios may influence the temperature at which menthol is released from the amorphous solid when heated.
- Providing a gelling agent which comprises more alginate than pectin may be advantageous due to lower material costs. However, a gelling agent comprising alginate alone may have a high viscosity, meaning that it is difficult to process the gelling agent during the manufacture of the amorphous solid. The inventors have identified that, by combining alginate with pectin wherein pectin is present as a minority portion, the viscosity of the gelling agent may be easier to process during the manufacture of the amorphous solid.
- In some embodiments, the pectin is comprised in the gelling agent in an amount of from 3-10wt% of the amorphous solid. That is, the amorphous solid comprises pectin in an amount of 3-10wt% by dry weight of the amorphous solid. In some embodiments, the amorphous solid comprises pectin in an amount of from 3-8wt%, or 4wt% to 6wt%.
- Suitably, the amorphous solid comprises from about 1wt%, 5wt%, 10wt%, 15wt%, 20wt% or 25wt% to about 60wt%, 50wt%, 45wt%, 40wt%, 35wt%, 30wt% or 27wt% of gelling agent (all calculated on a dry weight basis). For example, the amorphous solid may comprise 1-50wt%, 5-40wt%, or 25-3 5wt% of a gelling agent.
- In some embodiments, the gelling agent further comprises a hydrocolloid other than those mentioned above. In some embodiments, the gelling agent further comprises one or more compounds selected from the group comprising starches (and derivatives), celluloses (and derivatives, such as such as methylcellulose, hydroxypropyl cellulose, and carboxymethyl cellulose (CMC)), gums, silica or silicones compounds, clays, polyvinyl alcohol and combinations thereof. For example, in some embodiments, the gelling agent further comprises one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose, pullulan, xanthan gum, guar gum, carrageenan, agarose, acacia gum, fumed silica, PDMS, sodium silicate, kaolin and polyvinyl alcohol.
- The gelling agent may further comprise one or more compounds selected from cellulosic gelling agents, non-cellulosic gelling agents, guar gum, acacia gum and mixtures thereof.
- In some embodiments, the cellulosic gelling agent is selected from the group consisting of: hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose (CMC), hydroxypropyl methylcellulose (HPMC), methyl cellulose, ethyl cellulose, cellulose acetate (CA), cellulose acetate butyrate (CAB), cellulose acetate propionate (CAP) and combinations thereof.
- In some embodiments, the gelling agent further comprises one or more of hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose (HPMC), carboxymethylcellulose, guar gum, or acacia gum.
- In some embodiments, the gelling agent further comprises one or more non-cellulosic gelling agents, including, but not limited to, agar, xanthan gum, gum Arabic, guar gum, locust bean gum, carrageenan, starch, and combinations thereof. In preferred embodiments, the non-cellulose based gelling agent further comprises agar.
- The aerosol-generating material comprises menthol in an amount of from 0.1-80wt%. In some embodiments, the aerosol-generating material comprises menthol in an amount of from about 1wt%, 5wt%, 10wt%, 15wt%, 20wt% or 25wt% to about 70wt%, 50wt%, 45wt% or 40wt% (calculated on a dry weight basis). In particular embodiments, the amorphous solid comprises 10-60wt%, 40-60wt% or 45-55wt% of menthol.
- The amorphous solid comprises 0.1-50wt% aerosol-former material. In some embodiments, the amorphous solid comprises 10-30wt% aerosol-former material, or 15-25wt% aerosol-former material.
- In some embodiments, the aerosol-former material may comprise one or more of glycerine, glycerol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,3-butylene glycol, erythritol, meso-Erythritol, ethyl vanillate, ethyl laurate, a diethyl suberate, triethyl citrate, triacetin, a diacetin mixture, benzyl benzoate, benzyl phenyl acetate, tributyrin, lauryl acetate, lauric acid, myristic acid, and propylene carbonate.
- In some embodiments, the aerosol former comprises one or more polyhydric alcohols, such as propylene glycol, triethylene glycol, 1 ,3-butanediol and glycerin; esters of polyhydric alcohols, such as glycerol mono-, di- or triacetate; and/or aliphatic esters of mono-, di- or polycarboxylic acids, such as dimethyl dodecanedioate and dimethyl tetradecanedioate.
- In an embodiment, the amorphous solid comprises:
- 20-3 5wt% of the gelling agent;
- 15-25wt% of the aerosol-former material;
- 45-55wt% of the menthol;
- The amorphous solid may have any suitable water content, such as from 1wt% to 15wt% (wet weight basis - "WWB"). Suitably, the water content of the amorphous solid may be from about 5wt%, 7wt% or 9wt% to about 15wt%, 13wt% or 11wt% (WWB).
- The aerosolisable or non-aerosol-generating material may be present on or in a support to form a substrate. The support functions as a support on which the amorphous solid layer forms, easing manufacture. The support may provide rigidity to the amorphous solid layer, easing handling.
- The support may be any suitable material which can be used to support an amorphous solid. In some cases, the support may be formed from materials selected from metal foil, paper, carbon paper, greaseproof paper, ceramic, carbon allotropes such as graphite and graphene, plastic, cardboard, wood or combinations thereof. In some cases, the support may comprise or consist of a tobacco material, such as a sheet of reconstituted tobacco. In some cases, the support may be formed from materials selected from metal foil, paper, cardboard, wood or combinations thereof. In some cases, the support comprises paper. In some cases, the support itself be a laminate structure comprising layers of materials selected from the preceding lists. In some cases, the support may also function as a flavour support. For example, the support may be impregnated with a flavourant or with tobacco extract.
- Suitably, the thickness of the support layer may be in the range of about 10µm, 15µm, 17µm, 20µm, 23µm, 25µm, 50µm, 75µm or 0.1mm to about 2.5mm, 2.0mm, 1.5mm, 1.0mm or 0.5mm. The support may comprise more than one layer, and the thickness described herein refers to the aggregate thickness of those layers.
- In some cases, the support may be magnetic. This functionality may be used to fasten the support to the assembly in use, or may be used to generate particular amorphous solid shapes. In some cases, the aerosol generating substrate may comprise one or more magnets which can be used to fasten the substrate to an induction heater in use.
- In some cases, the support may be substantially or wholly impermeable to gas and/or aerosol. This prevents aerosol or gas passage through the support layer, thereby controlling the flow and ensuring it is delivered to the user. This can also be used to prevent condensation or other deposition of the gas/aerosol in use on, for example, the surface of a heater provided in an aerosol generating assembly. Thus, consumption efficiency and hygiene can be improved in some cases.
- In some cases, the surface of the support that abuts the amorphous solid may be porous. For example, in one case, the support comprises paper. The inventors have found that a porous support such as paper is particularly suitable for the present invention; the porous (e.g. paper) layer abuts the amorphous solid layer and forms a strong bond. The amorphous solid is formed by drying a gel and, without being limited by theory, it is thought that the slurry from which the gel is formed partially impregnates the porous support (e.g. paper) so that when the gel sets and forms cross-links, the support is partially bound into the gel. This provides a strong binding between the gel and the support (and between the dried gel and the support).
- Additionally, surface roughness may contribute to the strength of bond between the amorphous material and the support. The inventors have found that the paper roughness (for the surface abutting the support) may suitably be in the range of 50-1000 Bekk seconds, suitably 50-150 Bekk seconds, suitably 100 Bekk seconds (measured over an air pressure interval of 50.66-48.00 kPa). (A Bekk smoothness tester is an instrument used to determine the smoothness of a paper surface, in which air at a specified pressure is leaked between a smooth glass surface and a paper sample, and the time (in seconds) for a fixed volume of air to seep between these surfaces is the "Bekk smoothness".)
- Conversely, the surface of the support facing away from the amorphous solid may be arranged in contact with the heater, and a smoother surface may provide more efficient heat transfer. Thus, in some cases, the support is disposed so as to have a rougher side abutting the amorphous material and a smoother side facing away from the amorphous material.
- In one particular case, the support may be a paper-backed foil; the paper layer abuts the amorphous solid layer and the properties discussed in the previous paragraphs are afforded by this abutment. The foil backing is substantially impermeable, providing control of the aerosol flow path. A metal foil backing may also serve to conduct heat to the amorphous solid.
- In another case, the foil layer of the paper-backed foil abuts the amorphous solid. The foil is substantially impermeable, thereby preventing water provided in the amorphous solid to be absorbed into the paper which could weaken its structural integrity.
- In some cases, the support is formed from or comprises metal foil, such as aluminium foil. A metallic support may allow for better conduction of thermal energy to the amorphous solid. Additionally, or alternatively, a metal foil may function as a susceptor in an induction heating system. In particular embodiments, the support comprises a metal foil layer and a support layer, such as cardboard. In these embodiments, the metal foil layer may have a thickness of less than 20µm, such as from about 1µm to about 10µm, suitably about 5µm.
- In some cases, the support may have a thickness of between about 0.017mm and about 2.0mm, suitably from about 0.02mm, 0.05mm or 0.1mm to about 1.5mm, 1.0mm, or 0.5mm.
- In some cases, the aerosol generating substrate may comprise embedded heating means, such as resistive or inductive heating elements. For example, the heating means may be embedded in the amorphous solid.
- The amorphous solid may be made from a gel, and this gel may additionally comprise a solvent, included at 0.1-50wt%. However, the inventors have established that the inclusion of a solvent in which the flavour is soluble may reduce the gel stability and the flavour may crystallise out of the gel. As such, in some cases, the gel does not include a solvent in which the flavour is soluble.
- In some embodiments, the amorphous solid comprises less than 60wt% of a filler, such as from 1wt% to 60wt%, or 5wt% to 50wt%, or 5wt% to 30wt%, or 10wt% to 20wt%.
- In other embodiments, the amorphous solid comprises less than 20wt%, suitably less than 10wt% or less than 5wt% of a filler. In some cases, the amorphous solid comprises less than 1wt% of a filler, and in some cases, comprises no filler.
- An aspect of the present invention relates to an article. A consumable is an article, part or all of which is intended to be consumed during use by a user. A consumable may comprise or consist of aerosol-generating material. A consumable may comprise one or more other elements, such as a filter or an aerosol modifying substance. A consumable may comprise a heating element that emits heat to cause the aerosol-generating material to generate aerosol in use. The heating element may, for example, comprise combustible material, or may comprise a susceptor that is heatable by penetration with a varying magnetic field.
- Articles of the present invention may be provided in any suitable shape. In some examples, the article is provided as a rod (e.g. substantially cylindrical). An article provided as a rod may include the aerosol-generating material as a shredded sheet, optionally blended with cut tobacco. Alternatively, or additionally, the article provided as a rod may include the aerosol-generating material as a sheet, such as a sheet circumscribing a rod of aerosol-generating material (e.g. tobacco). In some embodiments, the article comprises a layer portion of aerosol-generating material disposed on a carrier. In examples, the article may have at least one substantially planar (flat) surface.
- A susceptor is material that is heatable by penetration with a varying magnetic field, such as an alternating magnetic field. The heating material may be an electrically-conductive material, so that penetration thereof with a varying magnetic field causes induction heating of the heating material. The heating material may be magnetic material, so that penetration thereof with a varying magnetic field causes magnetic hysteresis heating of the heating material. The heating material may be both electrically-conductive and magnetic, so that the heating material is heatable by both heating mechanisms.
- Induction heating is a process in which an electrically-conductive object is heated by penetrating the object with a varying magnetic field. The process is described by Faraday's law of induction and Ohm's law. An induction heater may comprise an electromagnet and a device for passing a varying electrical current, such as an alternating current, through the electromagnet. When the electromagnet and the object to be heated are suitably relatively positioned so that the resultant varying magnetic field produced by the electromagnet penetrates the object, one or more eddy currents are generated inside the object. The object has a resistance to the flow of electrical currents. Therefore, when such eddy currents are generated in the object, their flow against the electrical resistance of the object causes the obj ect to be heated. This process is called Joule, ohmic, or resistive heating.
- In some embodiments, the susceptor is in the form of a closed circuit. It has been found that, when the susceptor is in the form of a closed circuit, magnetic coupling between the susceptor and the electromagnet in use is enhanced, which results in greater or improved Joule heating.
- Magnetic hysteresis heating is a process in which an object made of a magnetic material is heated by penetrating the object with a varying magnetic field. A magnetic material can be considered to comprise many atomic-scale magnets, or magnetic dipoles. When a magnetic field penetrates such material, the magnetic dipoles align with the magnetic field. Therefore, when a varying magnetic field, such as an alternating magnetic field, for example as produced by an electromagnet, penetrates the magnetic material, the orientation of the magnetic dipoles changes with the varying applied magnetic field. Such magnetic dipole reorientation causes heat to be generated in the magnetic material.
- When an object is both electrically-conductive and magnetic, penetrating the object with a varying magnetic field can cause both Joule heating and magnetic hysteresis heating in the object. Moreover, the use of magnetic material can strengthen the magnetic field, which can intensify the Joule heating.
- In each of the above processes, as heat is generated inside the object itself, rather than by an external heat source by heat conduction, a rapid temperature rise in the object and more uniform heat distribution can be achieved, particularly through selection of suitable object material and geometry, and suitable varying magnetic field magnitude and orientation relative to the object. Moreover, as induction heating and magnetic hysteresis heating do not require a physical connection to be provided between the source of the varying magnetic field and the object, design freedom and control over the heating profile may be greater, and cost may be lower.
- The filler, if present, may comprise one or more inorganic filler materials, such as calcium carbonate, perlite, vermiculite, diatomaceous earth, colloidal silica, magnesium oxide, magnesium sulphate, magnesium carbonate, and suitable inorganic sorbents, such as molecular sieves. The filler may comprise one or more organic filler materials such as wood pulp, cellulose and cellulose derivatives. In particular cases, the amorphous solid comprises no calcium carbonate such as chalk.
- In particular embodiments which include filler, the filler is fibrous. For example, the filler may be a fibrous organic filler material such as wood pulp, hemp fibre, cellulose or cellulose derivatives. Without wishing to be bound by theory, it is believed that including fibrous filler in an amorphous solid may increase the tensile strength of the material. This may be particularly advantageous in examples wherein the amorphous solid is provided as a sheet, such as when an amorphous solid sheet circumscribes a rod of aerosol-generating material.
- In some embodiments, the amorphous solid does not comprise tobacco fibres. In particular embodiments, the amorphous solid does not comprise fibrous material.
- In some embodiments, the aerosol generating material does not comprise tobacco fibres. In particular embodiments, the aerosol generating material does not comprise fibrous material.
- In some embodiments, the aerosol-generating material does not comprise tobacco fibres. In particular embodiments, the aerosol-generating material does not comprise fibrous material.
- In some embodiments, the aerosol-generating article does not comprise tobacco fibres. In particular embodiments, the aerosol-generating article does not comprise fibrous material.
- In some cases, the amorphous solid may consist essentially of, or consist of a gelling agent, an aerosol generating agent, water, and menthol.
- In some embodiments, the aerosol-generating material, or amorphous solid, comprises one or more cannabinoid compounds selected from the group consisting of cannabidiol (CBD), tetrahydrocannabinol (THC), tetrahydrocannabinolic acid (THCA), cannabidiolic acid (CBDA), cannabinol (CBN), cannabigerol (CBG), cannabichromene (CBC), cannabicyclol (CBL), cannabivarin (CBV), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), cannabichromevarin (CBCV), cannabigerovarin (CBGV), cannabigerol monomethyl ether (CBGM) and cannabielsoin (CBE), cannabicitran (CBT).
- The aerosol-generating material, or amorphous solid, may comprise one or more cannabinoid compounds selected from the group consisting of cannabidiol (CBD) and THC (tetrahydrocannabinol).
- The aerosol-generating material, or amorphous solid, may comprise cannabidiol (CBD).
- The aerosol-generating material, or amorphous solid, may comprise nicotine and cannabidiol (CBD).
- The aerosol-generating material, or amorphous solid, may comprise nicotine, cannabidiol (CBD), and THC (tetrahydrocannabinol).
- The aerosol generating material comprising the amorphous solid may have any suitable area density, such as from 30 g/m2 to 120 g/m2. In some embodiments, aerosol generating material may have an area density of from about 30 to 70 g/m2, or about 40 to 60 g/m2. In some embodiments, the amorphous solid may have an area density of from about 80 to 120 g/m2, or from about 70 to 110 g/m2, or particularly from about 90 to 110 g/m2. Such area densities may be particularly suitable where the aerosol-generating material is included in an aerosol-generating article/assembly in sheet form, or as a shredded sheet (described further hereinbelow).
- An aspect of the invention provides non-combustible aerosol provision system comprising an article according as described herein and non-combustible aerosol provision device comprising a heater which is configured to heat not burn the aerosol-generating article. A non-combustible aerosol provision system may also be referred to as an aerosol generating assembly. A non-combustible aerosol provision device may be referred to as an aerosol generating apparatus.
- In some cases, in use, the heater may heat, without burning, the aerosol-generating material to a temperature of less than 350 °C, such as between 120°C and 350 °C. In some cases, the heater may heat, without burning, the aerosol-generating material to between 140 °C and 250 °C in use, or between 220 °C and 280 °C. In some cases in use, substantially all of the amorphous solid is less than about 4mm, 3mm, 2mm or 1mm from the heater. In some cases, the solid is disposed between about 0.010mm and 2.0mm from the heater, suitably between about 0.02mm and 1.0mm, suitably 0.1mm to 0.5mm. These minimum distances may, in some cases, reflect the thickness of a support that supports the amorphous solid. In some cases, a surface of the amorphous solid may directly abut the heater.
- The heater is configured to heat not burn the aerosol-generating article, and thus the aerosol-generating material. The heater may be, in some cases, a thin film, electrically resistive heater. In other cases, the heater may comprise an induction heater or the like. The heater may be a combustible heat source or a chemical heat source which undergoes an exothermic reaction to product heat in use. The aerosol generating assembly may comprise a plurality of heaters. The heater(s) may be powered by a battery.
- The aerosol-generating article may additionally comprise a cooling element and/or a filter. The cooling element, if present, may act or function to cool gaseous or aerosol components. In some cases, it may act to cool gaseous components such that they condense to form an aerosol. It may also act to space the very hot parts of the non-combustible aerosol provision device from the user. The filter, if present, may comprise any suitable filter known in the art such as a cellulose acetate plug.
- In some cases, the aerosol generating assembly may be a heat-not-burn device. That is, it may contain a solid tobacco-containing material (and no liquid aerosol-generating material). In some cases, the amorphous solid may comprise the tobacco material. A heat-not-burn device is disclosed in
WO 2015/062983 A2 , which is incorporated by reference in its entirety. - In some cases, the aerosol generating assembly may be an electronic tobacco hybrid device. That is, it may contain a solid aerosol-generating material and a liquid aerosol-generating material. In some cases, the amorphous solid may comprise nicotine. In some cases, the amorphous solid may comprise a tobacco material. In some cases, the amorphous solid may comprise a tobacco material and a separate nicotine source. The separate aerosol-generating materials may be heated by separate heaters, the same heater or, in one case, a downstream aerosol-generating material may be heated by a hot aerosol which is generated from the upstream aerosol-generating material. An electronic tobacco hybrid device is disclosed in
WO 2016/135331 A1 , which is incorporated by reference in its entirety. - The aerosol-generating material or amorphous solid may comprise an acid. The acid may be an organic acid. In some of these embodiments, the acid may be at least one of a monoprotic acid, a diprotic acid and a triprotic acid. In some such embodiments, the acid may contain at least one carboxyl functional group. In some such embodiments, the acid may be at least one of an alpha-hydroxy acid, carboxylic acid, dicarboxylic acid, tricarboxylic acid and keto acid. In some such embodiments, the acid may be an alpha-keto acid.
- In some such embodiments, the acid may be at least one of succinic acid, lactic acid, benzoic acid, citric acid, tartaric acid, fumaric acid, levulinic acid, acetic acid, malic acid, formic acid, sorbic acid, benzoic acid, propanoic and pyruvic acid.
- Suitably the acid is lactic acid. In other embodiments, the acid is benzoic acid. In other embodiments the acid may be an inorganic acid. In some of these embodiments the acid may be a mineral acid. In some such embodiments, the acid may be at least one of sulphuric acid, hydrochloric acid, boric acid and phosphoric acid. In some embodiments, the acid is levulinic acid.
- The inclusion of an acid is particularly preferred in embodiments in which the aerosol-generating material or amorphous solid comprises nicotine. In such embodiments, the presence of an acid may stabilise dissolved species in the slurry from which the aerosol-generating material or amorphous solid is formed. The presence of the acid may reduce or substantially prevent evaporation of nicotine during drying of the slurry, thereby reducing loss of nicotine during manufacturing.
- The amorphous solid may comprise a colourant. The addition of a colourant may alter the visual appearance of the amorphous solid. The presence of colourant in the amorphous solid may enhance the visual appearance of the amorphous solid and the aerosol-generating material. By adding a colourant to the amorphous solid, the amorphous solid may be colour-matched to other components of the aerosol-generating material or to other components of an article comprising the amorphous solid.
- A variety of colourants may be used depending on the desired colour of the amorphous solid. The colour of amorphous solid may be, for example, white, green, red, purple, blue, brown or black. Other colours are also envisaged. Natural or synthetic colourants, such as natural or synthetic dyes, food-grade colourants and pharmaceutical-grade colourants may be used. In certain embodiments, the colourant is caramel, which may confer the amorphous solid with a brown appearance. In such embodiments, the colour of the amorphous solid may be similar to the colour of other components (such as tobacco material) in an aerosol-generating material comprising the amorphous solid. In some embodiments, the addition of a colourant to the amorphous solid renders it visually indistinguishable from other components in the aerosol-generating material.
- The colourant may be incorporated during the formation of the amorphous solid (e.g. when forming a slurry comprising the materials that form the amorphous solid) or it may be applied to the amorphous solid after its formation (e.g. by spraying it onto the amorphous solid).
- The aerosol-generating article (which may be referred to herein as an article, a cartridge or a consumable) may be adapted for use in a THP, an electronic tobacco hybrid device or another aerosol generating device. In some cases, the article may additionally comprise a filter and/or cooling element (which have been described above). In some cases, the aerosol-generating article may be circumscribed by a wrapping material such as paper.
- The aerosol-generating article may additionally comprise ventilation apertures. These may be provided in the sidewall of the article. In some cases, the ventilation apertures may be provided in the filter and/or cooling element. These apertures may allow cool air to be drawn into the article during use, which can mix with the heated volatilised components thereby cooling the aerosol.
- The ventilation enhances the generation of visible heated volatilised components from the article when it is heated in use. The heated volatilised components are made visible by the process of cooling the heated volatilised components such that supersaturation of the heated volatilised components occurs. The heated volatilised components then undergo droplet formation, otherwise known as nucleation, and eventually the size of the aerosol particles of the heated volatilised components increases by further condensation of the heated volatilised components and by coagulation of newly formed droplets from the heated volatilised components.
- In some cases, the ratio of the cool air to the sum of the heated volatilised components and the cool air, known as the ventilation ratio, is at least 15%. A ventilation ratio of 15% enables the heated volatilised components to be made visible by the method described above. The visibility of the heated volatilised components enables the user to identify that the volatilised components have been generated and adds to the sensory experience of the smoking experience.
- In another example, the ventilation ratio is between 50% and 85% to provide additional cooling to the heated volatilised components. In some cases, the ventilation ratio may be at least 60% or 65%.
- In some cases, the aerosol generating material may be included in the article/assembly in sheet form. In some cases, the aerosol generating material may be included as a planar sheet. In some cases, the aerosol generating material may be included as a planar sheet, as a bunched or gathered sheet, as a crimped sheet, or as a rolled sheet (i.e. in the form of a tube). In some such cases, the amorphous solid of these embodiments may be included in an aerosol-generating article/assembly as a sheet, such as a sheet circumscribing a rod of aerosol-generating material (e.g. tobacco). In some other cases, the aerosol generating material may be formed as a sheet and then shredded and incorporated into the article. In some cases, the shredded sheet may be mixed with cut rag tobacco and incorporated into the article.
- In some examples, the amorphous solid in sheet form may have a tensile strength of from around 200 N/m to around 900 N/m. In some examples, such as where the amorphous solid does not comprise a filler, the amorphous solid may have a tensile strength of from 200 N/m to 400 N/m, or 200 N/m to 300 N/m, or about 250 N/m. Such tensile strengths may be particularly suitable for embodiments wherein the aerosol generating material is formed as a sheet and then shredded and incorporated into an aerosol-generating article. In some examples, such as where the amorphous solid comprises a filler, the amorphous solid may have a tensile strength of from 600 N/m to 900 N/m, or from 700 N/m to 900 N/m, or around 800 N/m. Such tensile strengths may be particularly suitable for embodiments wherein the aerosol generating material is included in an aerosol-generating article/assembly as a rolled sheet, suitably in the form of a tube.
- The assembly may comprise an integrated aerosol-generating article and heater, or may comprise a heater device into which the article is inserted in use.
- Referring to
Figures 1 and 2 , there are shown a partially cut-away section view and a perspective view of an example of an aerosol-generatingarticle 101. Thearticle 101 is adapted for use with a device having a power source and a heater. Thearticle 101 of this embodiment is particularly suitable for use with the device 51 shown inFigures 5 to 7 , described below. In use, thearticle 101 may be removably inserted into the device shown inFigure 5 at aninsertion point 20 of the device 51. - The
article 101 of one example is in the form of a substantially cylindrical rod that includes a body ofaerosol generating material 103 and afilter assembly 105 in the form of a rod. The aerosol generating material comprises the amorphous solid material described herein. In some embodiments, it may be included in sheet form. In some embodiments it may be included in the form of a shredded sheet. In some embodiments, the aerosol generating material described herein may be incorporated in sheet form and in shredded form. - The
filter assembly 105 includes three segments, acooling segment 107, afilter segment 109 and amouth end segment 111. Thearticle 101 has afirst end 113, also known as a mouth end or a proximal end and asecond end 115, also known as a distal end. The body ofaerosol generating material 103 is located towards thedistal end 115 of thearticle 101. In one example, thecooling segment 107 is located adjacent the body ofaerosol generating material 103 between the body ofaerosol generating material 103 and thefilter segment 109, such that thecooling segment 107 is in an abutting relationship with theaerosol generating material 103 and thefilter segment 103. In other examples, there may be a separation between the body ofaerosol generating material 103 and thecooling segment 107 and between the body ofaerosol generating material 103 and thefilter segment 109. Thefilter segment 109 is located in between the coolingsegment 107 and themouth end segment 111. Themouth end segment 111 is located towards theproximal end 113 of thearticle 101, adjacent thefilter segment 109. In one example, thefilter segment 109 is in an abutting relationship with themouth end segment 111. In one embodiment, the total length of thefilter assembly 105 is between 37mm and 45mm, more preferably, the total length of thefilter assembly 105 is 41mm. - In one example, the rod of
aerosol generating material 103 is between 34mm and 50mm in length, suitably between 38mm and 46mm in length, suitably 42mm in length. - In one example, the total length of the
article 101 is between 71mm and 95mm, suitably between 79mm and 87mm, suitably 83mm. - An axial end of the body of
aerosol generating material 103 is visible at thedistal end 115 of thearticle 101. However, in other embodiments, thedistal end 115 of thearticle 101 may comprise an end member (not shown) covering the axial end of the body ofaerosol generating material 103. - The body of
aerosol generating material 103 is joined to thefilter assembly 105 by annular tipping paper (not shown), which is located substantially around the circumference of thefilter assembly 105 to surround thefilter assembly 105 and extends partially along the length of the body ofaerosol generating material 103. In one example, the tipping paper is made of 58GSM standard tipping base paper. In one example the tipping paper has a length of between 42mm and 50mm, suitably of 46mm. - In one example, the
cooling segment 107 is an annular tube and is located around and defines an air gap within the cooling segment. The air gap provides a chamber for heated volatilised components generated from the body ofaerosol generating material 103 to flow. Thecooling segment 107 is hollow to provide a chamber for aerosol accumulation yet rigid enough to withstand axial compressive forces and bending moments that might arise during manufacture and whilst thearticle 101 is in use during insertion into the device 51. In one example, the thickness of the wall of thecooling segment 107 is approximately 0.29mm. - The
cooling segment 107 provides a physical displacement between theaerosol generating material 103 and thefilter segment 109. The physical displacement provided by thecooling segment 107 will provide a thermal gradient across the length of thecooling segment 107. In one example thecooling segment 107 is configured to provide a temperature differential of at least 40 degrees Celsius between a heated volatilised component entering a first end of thecooling segment 107 and a heated volatilised component exiting a second end of thecooling segment 107. In one example thecooling segment 107 is configured to provide a temperature differential of at least 60 degrees Celsius between a heated volatilised component entering a first end of thecooling segment 107 and a heated volatilised component exiting a second end of thecooling segment 107. This temperature differential across the length of thecooling element 107 protects the temperaturesensitive filter segment 109 from the high temperatures of theaerosol generating material 103 when it is heated by the device 51. If the physical displacement was not provided between thefilter segment 109 and the body ofaerosol generating material 103 and the heating elements of the device 51, then the temperature sensitive filter segment may 109 become damaged in use, so it would not perform its required functions as effectively. - In one example the length of the
cooling segment 107 is at least 15mm. In one example, the length of thecooling segment 107 is between 20mm and 30mm, more particularly 23mm to 27mm, more particularly 25mm to 27mm, suitably 25mm. - The
cooling segment 107 is made of paper, which means that it is comprised of a material that does not generate compounds of concern, for example, toxic compounds when in use adjacent to the heater of the device 51. In one example, thecooling segment 107 is manufactured from a spirally wound paper tube which provides a hollow internal chamber yet maintains mechanical rigidity. Spirally wound paper tubes are able to meet the tight dimensional accuracy requirements of high-speed manufacturing processes with respect to tube length, outer diameter, roundness and straightness. - In another example, the
cooling segment 107 is a recess created from stiff plug wrap or tipping paper. The stiff plug wrap or tipping paper is manufactured to have a rigidity that is sufficient to withstand the axial compressive forces and bending moments that might arise during manufacture and whilst thearticle 101 is in use during insertion into the device 51. - The
filter segment 109 may be formed of any filter material sufficient to remove one or more volatilised compounds from heated volatilised components from the aerosol generating material. In one example thefilter segment 109 is made of a mono-acetate material, such as cellulose acetate. Thefilter segment 109 provides cooling and irritation-reduction from the heated volatilised components without depleting the quantity of the heated volatilised components to an unsatisfactory level for a user. - In some embodiments, a capsule (not illustrated) may be provided in
filter segment 109. It may be disposed substantially centrally in thefilter segment 109, both across thefilter segment 109 diameter and along thefilter segment 109 length. In other cases, it may be offset in one or more dimension. The capsule may in some cases, where present, contain a volatile component such as a flavourant or aerosol generating agent. - The density of the cellulose acetate tow material of the
filter segment 109 controls the pressure drop across thefilter segment 109, which in turn controls the draw resistance of thearticle 101. Therefore the selection of the material of thefilter segment 109 is important in controlling the resistance to draw of thearticle 101. In addition, the filter segment performs a filtration function in thearticle 101. - In one example, the
filter segment 109 is made of a 8Y15 grade of filter tow material, which provides a filtration effect on the heated volatilised material, whilst also reducing the size of condensed aerosol droplets which result from the heated volatilised material. - The presence of the
filter segment 109 provides an insulating effect by providing further cooling to the heated volatilised components that exit thecooling segment 107. This further cooling effect reduces the contact temperature of the user's lips on the surface of thefilter segment 109. - In one example, the
filter segment 109 is between 6mm to 10mm in length, suitably 8mm. - The
mouth end segment 111 is an annular tube and is located around and defines an air gap within themouth end segment 111. The air gap provides a chamber for heated volatilised components that flow from thefilter segment 109. Themouth end segment 111 is hollow to provide a chamber for aerosol accumulation yet rigid enough to withstand axial compressive forces and bending moments that might arise during manufacture and whilst the article is in use during insertion into the device 51. In one example, the thickness of the wall of themouth end segment 111 is approximately 0.29mm. In one example, the length of themouth end segment 111 is between 6mm to 10mm, suitably 8mm. - The
mouth end segment 111 may be manufactured from a spirally wound paper tube which provides a hollow internal chamber yet maintains critical mechanical rigidity. Spirally wound paper tubes are able to meet the tight dimensional accuracy requirements of high-speed manufacturing processes with respect to tube length, outer diameter, roundness and straightness. - The
mouth end segment 111 provides the function of preventing any liquid condensate that accumulates at the exit of thefilter segment 109 from coming into direct contact with a user. - It should be appreciated that, in one example, the
mouth end segment 111 and thecooling segment 107 may be formed of a single tube and thefilter segment 109 is located within that tube separating themouth end segment 111 and thecooling segment 107. - Referring to
Figures 3 and 4 , there are shown a partially cut-away section and perspective views of an example of anarticle 301. The reference signs shown inFigures 3 and 4 are equivalent to the reference signs shown inFigures 1 and 2 , but with an increment of 200. - In the example of the
article 301 shown inFigures 3 and 4 , aventilation region 317 is provided in thearticle 301 to enable air to flow into the interior of thearticle 301 from the exterior of thearticle 301. In one example theventilation region 317 takes the form of one or more ventilation holes 317 formed through the outer layer of thearticle 301. The ventilation holes may be located in thecooling segment 307 to aid with the cooling of thearticle 301. In one example, theventilation region 317 comprises one or more rows of holes, and preferably, each row of holes is arranged circumferentially around thearticle 301 in a cross-section that is substantially perpendicular to a longitudinal axis of thearticle 301. - In one example, there are between one to four rows of ventilation holes to provide ventilation for the
article 301. Each row of ventilation holes may have between 12 to 36 ventilation holes 317. The ventilation holes 317 may, for example, be between 100 to 500µm in diameter. In one example, an axial separation between rows of ventilation holes 317 is between 0.25mm and 0.75mm, suitably 0.5mm. - In one example, the ventilation holes 317 are of uniform size. In another example, the ventilation holes 317 vary in size. The ventilation holes can be made using any suitable technique, for example, one or more of the following techniques: laser technology, mechanical perforation of the
cooling segment 307 or pre-perforation of thecooling segment 307 before it is formed into thearticle 301. The ventilation holes 317 are positioned so as to provide effective cooling to thearticle 301. - In one example, the rows of
ventilation holes 317 are located at least 11mm from theproximal end 313 of the article, suitably between 17mm and 20mm from theproximal end 313 of thearticle 301. The location of the ventilation holes 317 is positioned such that user does not block the ventilation holes 317 when thearticle 301 is in use. - Providing the rows of ventilation holes between 17mm and 20mm from the
proximal end 313 of thearticle 301 enables the ventilation holes 317 to be located outside of the device 51, when thearticle 301 is fully inserted in the device 51, as can be seen inFigures 6 and7 . By locating the ventilation holes outside of the device, non-heated air is able to enter thearticle 301 through the ventilation holes from outside the device 51 to aid with the cooling of thearticle 301. - The length of the
cooling segment 307 is such that thecooling segment 307 will be partially inserted into the device 51, when thearticle 301 is fully inserted into the device 51. The length of thecooling segment 307 provides a first function of providing a physical gap between the heater arrangement of the device 51 and the heatsensitive filter arrangement 309, and a second function of enabling the ventilation holes 317 to be located in the cooling segment, whilst also being located outside of the device 51, when thearticle 301 is fully inserted into the device 51. As can be seen fromFigures 6 and7 , the majority of thecooling element 307 is located within the device 51. However, there is a portion of thecooling element 307 that extends out of the device 51. It is in this portion of thecooling element 307 that extends out of the device 51 in which the ventilation holes 317 are located. - Referring now to
Figures 5 to 7 in more detail, there is shown an example of a device 51 arranged to heat aerosol generating material to volatilise at least one component of said aerosol generating material, typically to form an aerosol which can be inhaled. The device 51 is a heating device which releases compounds by heating, but not burning, the aerosol generating material. - A first end 53 is sometimes referred to herein as the mouth or proximal end 53 of the device 51 and a second end 55 is sometimes referred to herein as the distal end 55 of the device 51. The device 51 has an on/off button 57 to allow the device 51 as a whole to be switched on and off as desired by a user.
- The device 51 comprises a housing 59 for locating and protecting various internal components of the device 51. In the example shown, the housing 59 comprises a
uni-body sleeve 11 that encompasses the perimeter of the device 51, capped with atop panel 17 which defines generally the 'top' of the device 51 and abottom panel 19 which defines generally the 'bottom' of the device 51. In another example the housing comprises a front panel, a rear panel and a pair of opposite side panels in addition to thetop panel 17 and thebottom panel 19. - The
top panel 17 and/or thebottom panel 19 may be removably fixed to theuni-body sleeve 11, to permit easy access to the interior of the device 51, or may be "permanently" fixed to theuni-body sleeve 11, for example to deter a user from accessing the interior of the device 51. In an example, thepanels uni-body sleeve 11 is made of aluminium, though other materials and other manufacturing processes may be used. - The
top panel 17 of the device 51 has anopening 20 at the mouth end 53 of the device 51 through which, in use, thearticle - The housing 59 has located or fixed therein a
heater arrangement 23,control circuitry 25 and apower source 27. In this example, theheater arrangement 23, thecontrol circuitry 25 and thepower source 27 are laterally adjacent (that is, adjacent when viewed from an end), with thecontrol circuitry 25 being located generally between theheater arrangement 23 and thepower source 27, though other locations are possible. - The
control circuitry 25 may include a controller, such as a microprocessor arrangement, configured and arranged to control the heating of the aerosol generating material in thearticle - The
power source 27 may be for example a battery, which may be a rechargeable battery or a non-rechargeable battery. Examples of suitable batteries include for example a lithium-ion battery, a nickel battery (such as a nickel-cadmium battery), an alkaline battery and/ or the like. Thebattery 27 is electrically coupled to theheater arrangement 23 to supply electrical power when required and under control of thecontrol circuitry 25 to heat the aerosol generating material in the article (as discussed, to volatilise the aerosol generating material without causing the aerosol generating material to burn). - An advantage of locating the
power source 27 laterally adjacent to theheater arrangement 23 is that a physicallylarge power source 25 may be used without causing the device 51 as a whole to be unduly lengthy. As will be understood, in general a physicallylarge power source 25 has a higher capacity (that is, the total electrical energy that can be supplied, often measured in Amp-hours or the like) and thus the battery life for the device 51 can be longer. - In one example, the
heater arrangement 23 is generally in the form of a hollow cylindrical tube, having a hollow interior heating chamber 29 into which thearticle heater arrangement 23 are possible. For example, theheater arrangement 23 may comprise a single heating element or may be formed of plural heating elements aligned along the longitudinal axis of theheater arrangement 23. The or each heating element may be annular or tubular, or at least part-annular or part-tubular around its circumference. In an example, the or each heating element may be a thin film heater. In another example, the or each heating element may be made of a ceramics material. Examples of suitable ceramics materials include alumina and aluminium nitride and silicon nitride ceramics, which may be laminated and sintered. Other heating arrangements are possible, including for example inductive heating, infrared heater elements, which heat by emitting infrared radiation, or resistive heating elements formed by for example a resistive electrical winding. - In one particular example, the
heater arrangement 23 is supported by a stainless steel support tube and comprises a polyimide heating element. Theheater arrangement 23 is dimensioned so that substantially the whole of the body ofaerosol generating material article heater arrangement 23 when thearticle - The or each heating element may be arranged so that selected zones of the aerosol generating material can be independently heated, for example in turn (over time, as discussed above) or together (simultaneously) as desired.
- The
heater arrangement 23 in this example is surrounded along at least part of its length by athermal insulator 31. Theinsulator 31 helps to reduce heat passing from theheater arrangement 23 to the exterior of the device 51. This helps to keep down the power requirements for theheater arrangement 23 as it reduces heat losses generally. Theinsulator 31 also helps to keep the exterior of the device 51 cool during operation of theheater arrangement 23. In one example, theinsulator 31 may be a double-walled sleeve which provides a low pressure region between the two walls of the sleeve. That is, theinsulator 31 may be for example a "vacuum" tube, i.e. a tube that has been at least partially evacuated so as to minimise heat transfer by conduction and/or convection. Other arrangements for theinsulator 31 are possible, including using heat insulating materials, including for example a suitable foam-type material, in addition to or instead of a double-walled sleeve. - The housing 59 may further comprises various
internal support structures 37 for supporting all internal components, as well as theheating arrangement 23. - The device 51 further comprises a
collar 33 which extends around and projects from theopening 20 into the interior of the housing 59 and a generallytubular chamber 35 which is located between thecollar 33 and one end of thevacuum sleeve 31. Thechamber 35 further comprises acooling structure 35f, which in this example, comprises a plurality ofcooling fins 35f spaced apart along the outer surface of thechamber 35, and each arranged circumferentially around outer surface of thechamber 35. There is anair gap 36 between thehollow chamber 35 and thearticle hollow chamber 35. Theair gap 36 is around all of the circumference of thearticle cooling segment 307. - The
collar 33 comprises a plurality ofridges 60 arranged circumferentially around the periphery of theopening 20 and which project into theopening 20. Theridges 60 take up space within theopening 20 such that the open span of theopening 20 at the locations of theridges 60 is less than the open span of theopening 20 at the locations without theridges 60. Theridges 60 are configured to engage with anarticle ridges 60 and thearticle article article article air gap 36. - In operation, the
article insertion point 20 of the device 51, as shown inFigures 5 to 7 . Referring particularly toFigure 6 , in one example, the body ofaerosol generating material distal end article heater arrangement 23 of the device 51. Theproximal end article - In operation, the
heater arrangement 23 will heat thearticle aerosol generating material - The primary flow path for the heated volatilised components from the body of
aerosol generating material article cooling segment filter segment mouth end segment cooling segment cooling segment - In the examples of the
article 301 shown inFigures 3 and 4 , cool air will be able to enter thecooling segment 307 via the ventilation holes 317 formed in thecooling segment 307. This cool air will mix with the heated volatilised components to provide additional cooling to the heated volatilised components. - Another aspect of the invention provides a method of making an aerosol-generating material according to the first aspect, the method comprising (a) providing slurry comprising the gelling agent, aerosol-former material and menthol, (b) forming a layer of the slurry, (c) setting the slurry to form a gel, and (d) drying to form an amorphous solid.
- The (b) forming a layer the of the slurry may comprise spraying, casting or extruding the slurry, for example. In some cases, the slurry layer is formed by electrospraying the slurry. In some cases, the slurry layer is formed by casting the slurry.
- In some cases, the (b) and/or (c) and/or (d) may, at least partially, occur simultaneously (for example, during electrospraying). In some cases, (b), (c) and (d) may occur sequentially.
- In some cases, the slurry is applied to a support. The layer may be formed on a support.
- In examples, the slurry comprises gelling agent, aerosol-former material and menthol. The slurry may comprise these components in any of the proportions given herein in relation to the composition of the aerosol-generating material. For example, the slurry may comprise:
- 0.1-80 wt% of menthol;
- 1-60 wt% of a gelling agent / gelling agent precursor; and
- 0.1-50 wt% of an aerosol-former material.
- The slurry may comprise a gelling agent precursor. For example, the slurry may comprise sodium, potassium or ammonium alginate as a gel-precursor. In some embodiments, G units and M units are present in the gelling agent precursor in a molar ratio of from 1:2 to 10:1 (i.e. the number of α-(1-4)-linked L-guluronate units present compared with the number of β-(1-4)-linked D-mannuronate units). In some embodiments, the G units and M units are present in a molar ratio of from 1:3 to 3:1, or from 1:2 to 2:1, or from 1:1.5 to 1.5:1, or from 1:1.2 to 1.2:1.
- The setting the gel (c) may comprise the addition of a setting agent to the slurry. For example, (c) may comprise the addition of Ca2+ cations to the slurry. The Ca2+ cations may be provided as part of a calcium source. For example, the slurry may comprise sodium, potassium or ammonium alginate as a gel-precursor, and a setting agent comprising a calcium source (such as a calcium salt, e.g. calcium chloride), may be added to the slurry to form a calcium-crosslinked alginate gel. The Ca2+ calcium source is supplied to the slurry in an amount such that the molar ratio of Ca2+ cations to G units in the slurry is from 0.2:1 to 1:1, or from 0.3:1 to 0.5:1 or approximately 0.4:1 ("approximately" allowing for a 20% tolerance).
- In some embodiments the setting agent, or the calcium source, comprises or consists of calcium acetate, calcium formate, calcium carbonate, calcium hydrogencarbonate, calcium chloride, calcium lactate, or a combination thereof. In some examples, the setting agent, or the calcium source, comprises or consists of calcium formate and/or calcium lactate. In particular examples, the setting agent, or the calcium source, comprises or consists of calcium formate. The inventors have identified that, typically, employing calcium formate as a setting agent, or the calcium source, results in an amorphous solid having a greater tensile strength and greater resistance to elongation.
- In examples, Ca2+ cations are provided to the slurry as part of a fluid system comprising a calcium source and an aqueous carrier. The calcium source may comprise a combination of calcium-containing compounds. In some embodiments, the calcium source comprises one or more calcium salts such as calcium chloride, calcium lactate, calcium citrate, calcium acetate, or calcium citrate.
- In some examples, the calcium source is dissolved and optionally suspended in the aqueous carrier. In some examples, the calcium source is present in the fluid system in an amount which is greater than is soluble in the aqueous carrier under normal temperature and pressure. The normal temperature and pressure is as defined by the National Institute of Standards and Technology, and refers to a temperature of 20 °C and an absolute pressure of 1 atm.
- In some embodiments, the fluid source is a supersaturated solution of calcium source, such as a supersaturated solution of calcium salt(s). In some embodiments, the fluid source comprises dissolved and suspended (particulate) calcium source, such as dissolved and suspended (particulate) calcium salt. Providing the calcium source to the slurry in a small amount of aqueous carrier may reduce the evaporative load during the drying (d), thereby allowing for faster and less energy intensive production of the aerosol-generating material.
- The drying (d) may, in some cases, remove from about 50wt%, 60wt%, 70wt%, 80wt% or 90wt% to about 80wt%, 90wt% or 95wt% (WWB) of water in the slurry.
- The drying (d) may, in some cases, may reduce the cast material thickness by at least 80%, suitably 85% or 87%. For instance, the slurry may be cast at a thickness of 2mm, and the resulting dried amorphous solid material may have a thickness of 0.2mm.
- The slurry itself may also form part of the invention. In some cases, the slurry solvent may consist essentially of or consist of water. In some cases, the slurry may comprise from about 50wt%, 60wt%, 70wt%, 80wt% or 90wt% of solvent (WWB).
- In some examples, the slurry has a viscosity of from about 10 to about 20 Pa·s at 46.5 °C, such as from about 14 to about 16 Pa·s at 46.5 °C.
- In cases where the solvent consists of water, the dry weight content of the slurry may match the dry weight content of the amorphous solid. Thus, the discussion herein relating to the solid composition is explicitly disclosed in combination with the slurry aspect of the invention.
- According to an aspect of the present invention there is provided a method of generating an aerosol using a non-combustible aerosol provision system as described herein. In some embodiments, the method comprises heating the aerosol-generating material to a temperature of less than 350 °C. In some embodiments, the method comprises heating the aerosol-generating material to a temperature of from about 220 °C to about 280 °C. In some embodiments, the method comprises heating at least a portion of the aerosol-generating material to a temperature of from about 220 °C to about 280 °C over a session of use.
- "Session of use" as used herein refers to a single period of use of the non-combustible aerosol provision system by a user. The session of use begins at the point at which power is first supplied to at least one heating unit present in the heating assembly. The device will be ready for use after a period of time has elapsed from the start of the session of use. The session of use ends at the point at which no power is supplied to any of the heating elements in the aerosol-generating device. The end of the session of use may coincide with the point at which the smoking article is depleted (the point at which the total particulate matter yield (mg) in each puff would be deemed unacceptably low by a user). The session will have a duration of a plurality of puffs. Said session may have a duration less than 7 minutes, or 6 minutes, or 5 minutes, or 4 minutes and 30 seconds, or 4 minutes, or 3 minutes and 30 seconds. In some embodiments, the session of use may have a duration of from 2 to 5 minutes, or from 3 to 4.5 minutes, or 3.5 to 4.5 minutes, or suitably 4 minutes. A session may be initiated by the user actuating a button or switch on the device, causing at least one heating element to begin rising in temperature.
- In some embodiments, during a session of use, at least 20wt% of the menthol present in the amorphous solid is aerosolised, or at least 30wt%, 40wt% or 50wt%. That is, after a session of use, the amount of menthol in the amorphous solid is depleted by 20wt%, 30wt%, 40wt% or 50wt%. The molar ratio of Ca2+ to G units in the amorphous solid as described herein my allow for efficient delivery of menthol to a user (e.g. a high proportion of active material is aerosolised from the amorphous solid) whilst maintaining a long shelf-life before the amorphous solid is heated by the non-combustible aerosol provision device.
- A first aerosol-generating material and a second aerosol-generating material were prepared according to methods described herein. Both aerosol-generating materials were prepared from slurries having the following composition (w/w dry weight basis):
- 50% menthol
- 20% glycerol
- 26% sodium alginate
- 4% pectin
- Calcium lactate was supplied to the slurry as a setting agent. The aerosol-generating materials differed only in the amount of calcium lactate which was supplied to the slurry to cross-link the alginate. The first aerosol-generating material was prepared by supplying calcium lactate to the slurry in an amount such that the molar ratio of Ca2+ cations to G units in the sodium alginate was 0.4:1; the second aerosol-generating material was prepared by supplying calcium lactate to the slurry in an amount such that the molar ratio of Ca2+ cations to G units in the sodium alginate was 0.2:1.
- The dried material was formed as a sheet, which was subsequently shredded and combined with tobacco to provide a blend. Each blend of aerosol-generating material and tobacco was formed into a rod consumable and provided with a filter as described herein, providing a first consumable comprising the first aerosol-generating material and a second consumable comprising the second aerosol-generating material.
- Each consumable was subjected to sensory puff-by-puff analysis. The puff-by-puff analysis was carried out according to the Health Canada Intense (HCI) puffing regime: no vent blocking, 55mL puff over two seconds, every 30 seconds. Each puff was captured in a gas-tight syringe attached to a smoke engine. The captured sample was extracted with solvent and analysed with Gas Chromatography with Flame-Ionization Detection (GC-FID) for quantification of menthol against a calibration range.
-
Figure 8 depicts the results of this analysis. As can be seen, both materials give acceptable puff-by-puff menthol sensory performance. The first material, having a molar ratio of Ca2+ cations to G units of 0.4:1, was in particular found to provide desirable puff-by-puff menthol sensory performance. - The above embodiments are to be understood as illustrative examples of the invention. Further embodiments of the invention are envisaged. It is to be understood that any feature described in relation to any one embodiment may be used alone, or in combination with other features described, and may also be used in combination with one or more features of any other of the embodiments, or any combination of any other of the embodiments. Furthermore, equivalents and modifications not described above may also be employed without departing from the scope of the invention, which is defined in the accompanying claims.
Claims (17)
- An aerosol-generating material comprising an amorphous solid, the amorphous solid comprising:- 0.1-80 wt% of menthol;- 1-60 wt% of a gelling agent, the gelling agent comprising calcium-crosslinked alginate which comprises α-(1-4)-linked L-guluronate (G) units; and- 0.1-50 wt% of an aerosol-former material;wherein a molar ratio of Ca2+ cations to G units is from 0.2:1 to 1:1, preferably wherein the molar ratio of calcium to G units is from 0.3:1 to 0.5:1.
- The aerosol-generating material according to claim 1, wherein the calcium-crosslinked alginate also comprises β-(1-4)-linked D-mannuronate acid (M) units, preferably wherein a molar ratio of G units to M units is from 1:2 to 10:1.
- The aerosol-generating material according to claim 1 or 2 wherein, when stored for 30 days in a sealed container under ambient conditions (22 °C; 60% relative humidity; 1013 mbar), the aerosol-generating material contains at least 60% of the menthol by dry weight of the menthol present in the aerosol-generating material before storage.
- The aerosol-generating material according to any of claims 1 to 3, wherein the amorphous solid comprises the aerosol-former material in an amount of 10-30wt% and/or wherein the amorphous solid comprises the menthol in an amount of 40-60wt%.
- The aerosol-generating material according to any of claims 1 to 4, wherein the amorphous solid comprises:- 20-3 5wt% of the gelling agent;- 15-25wt% of the aerosol-former material;- 45-55wt% of the menthol;wherein these weights are calculated on a dry weight basis.
- The aerosol-generating material according to any of claims 1 to 5, wherein the cross-linked alginate comprised in the gelling agent is present in the amorphous solid in an amount of from about 15-40wt% of the amorphous solid on a dry weight basis.
- The aerosol-generating material according to any of claims 1 to 6, wherein the gelling agent further comprises pectin, preferably wherein a dry weight ratio of the cross-linked alginate to the pectin is from 1:1 to 10:1 and/or wherein the pectin comprised in the gelling agent is present in the amorphous solid in an amount of from about 3-10wt% of the amorphous solid on a dry weight basis.
- The aerosol-generating material according to any of claims 1 to 7, comprising from about 1wt% to about 15wt% of water (WWB).
- The aerosol-generating material according to any of claims 1 to 8, wherein the aerosol-former material is selected from erythritol, propylene glycol, glycerol and mixtures thereof.
- A substrate comprising an aerosol-generating material according to any of claims 1 to 9 and a support on which the aerosol-generating material is provided.
- An article for use with a non-combustible aerosol provision device, the article comprising an aerosol-generating material according to any one of claims 1 to 9 and/or a substrate according to claim 10.
- A non-combustible aerosol provision system comprising an article according to claim 11 and a non-combustible aerosol provision device, wherein the non-combustible aerosol provision device is configured to generate aerosol from the article when the article is used with the non-combustible aerosol provision device, wherein the non-combustible aerosol provision device comprises a heater configured to heat but not burn the article, preferably wherein the heater is configured to heat the article to a temperature of less than 350 °C in use, preferably from about 220 °C to about 280 °C in use.
- The system according to claim 12, wherein the article is provided as a rod.
- A method of making an aerosol-generating material according to any one of claims 1 to 9, the method comprising:- providing a slurry comprising the gelling agent, aerosol-former material and menthol;- forming a layer of the slurry;- setting the slurry to form a gel; and- drying the gel to form the amorphous solid.
- The method according to claim 14, wherein the setting the slurry comprises adding a calcium source comprising Ca2+ cations to the slurry, preferably wherein the calcium source is provided as part of a fluid system comprising the calcium source and an aqueous carrier, more preferably wherein the calcium source is dissolved and optionally suspended in the aqueous carrier, and/or wherein the calcium source is present in the fluid system in an amount which is greater than is soluble in the aqueous carrier under normal temperature and pressure.
- A method of generating an aerosol using a non-combustible aerosol provision system according to claim 12 or 13, the method comprising heating the aerosol-generating material to a temperature of less than 350 °C, preferably from about 220 °C to about 280 °C.
- The method according to claim 16 wherein, during a session of use, at least 20wt% of the menthol present in the amorphous solid is aerosolised.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GBGB1917472.1A GB201917472D0 (en) | 2019-11-29 | 2019-11-29 | Aerosol generation |
PCT/EP2020/083787 WO2021105465A1 (en) | 2019-11-29 | 2020-11-27 | Aerosol-generating material comprising an amorphous solid comprising methol and calcium-crosslinked alginate |
Publications (2)
Publication Number | Publication Date |
---|---|
EP4064866A1 EP4064866A1 (en) | 2022-10-05 |
EP4064866B1 true EP4064866B1 (en) | 2024-01-03 |
Family
ID=69147260
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP20816936.7A Active EP4064866B1 (en) | 2019-11-29 | 2020-11-27 | Aerosol-generating material comprising an amorphous solid comprising methol and calcium-crosslinked alginate |
Country Status (15)
Country | Link |
---|---|
US (1) | US20230024853A1 (en) |
EP (1) | EP4064866B1 (en) |
JP (1) | JP2023504250A (en) |
KR (1) | KR20220122607A (en) |
CN (1) | CN115243569A (en) |
AU (1) | AU2020391944A1 (en) |
BR (1) | BR112022010455A2 (en) |
CA (1) | CA3159870A1 (en) |
ES (1) | ES2969114T3 (en) |
GB (1) | GB201917472D0 (en) |
IL (1) | IL293172A (en) |
LT (1) | LT4064866T (en) |
PL (1) | PL4064866T3 (en) |
PT (1) | PT4064866T (en) |
WO (1) | WO2021105465A1 (en) |
Family Cites Families (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DK0419974T3 (en) * | 1989-09-29 | 1997-05-26 | Reynolds Tobacco Co R | Cigarette and smoky inserts therefor |
US5101839A (en) * | 1990-08-15 | 1992-04-07 | R. J. Reynolds Tobacco Company | Cigarette and smokable filler material therefor |
GB0324525D0 (en) * | 2003-10-21 | 2003-11-26 | British American Tobacco Co | Smoking articles and smokable filler material therefor |
GB0328644D0 (en) * | 2003-12-11 | 2004-01-14 | Souza Cruz Sa | Smoking article |
US20090038629A1 (en) * | 2007-08-07 | 2009-02-12 | Ergle J Dennis | Flavor sheet for smoking article |
US8663671B2 (en) * | 2009-11-05 | 2014-03-04 | Philip Morris Usa Inc. | Methods and compositions for producing hydrogel capsules coated for low permeability and physical integrity |
US10051884B2 (en) * | 2010-03-26 | 2018-08-21 | Philip Morris Usa Inc. | Controlled release mentholated tobacco beads |
AR081808A1 (en) * | 2010-03-26 | 2012-10-24 | Philip Morris Prod | PROCEDURE TO PRODUCE A CONTINUOUS STRUCTURE OF AN ENCAPSULATED MATERIAL |
GB201221376D0 (en) * | 2012-11-28 | 2013-01-09 | British American Tobacco Co | Controlling a smokeable material |
KR20220133303A (en) | 2013-10-29 | 2022-10-04 | 니코벤처스 트레이딩 리미티드 | Apparatus for heating smokable material |
GB201320231D0 (en) * | 2013-11-15 | 2014-01-01 | British American Tobacco Co | Aerosol generating material and devices including the same |
KR102370961B1 (en) * | 2013-12-31 | 2022-03-07 | 필립모리스 프로덕츠 에스.에이. | Smoking article with liquid delivery material |
EP3261467B1 (en) | 2015-02-27 | 2022-03-30 | Nicoventures Trading Limited | Cartridge, components and methods for generating an inhalable medium |
GB201508671D0 (en) * | 2015-05-20 | 2015-07-01 | British American Tobacco Co | Aerosol generating material and devices including the same |
US10334873B2 (en) * | 2016-06-16 | 2019-07-02 | Altria Client Services Llc | Breakable capsules and methods of forming thereof |
CN107723091B (en) * | 2017-11-29 | 2021-06-11 | 武汉黄鹤楼新材料科技开发有限公司 | Preparation method of mint essential oil blasting bead for cigarettes |
GB201812497D0 (en) * | 2018-07-31 | 2018-09-12 | Nicoventures Holdings Ltd | Aerosol generation |
GB201812501D0 (en) * | 2018-07-31 | 2018-09-12 | Nicoventures Trading Ltd | Aerosol generation |
-
2019
- 2019-11-29 GB GBGB1917472.1A patent/GB201917472D0/en not_active Ceased
-
2020
- 2020-11-27 AU AU2020391944A patent/AU2020391944A1/en active Pending
- 2020-11-27 ES ES20816936T patent/ES2969114T3/en active Active
- 2020-11-27 PT PT208169367T patent/PT4064866T/en unknown
- 2020-11-27 WO PCT/EP2020/083787 patent/WO2021105465A1/en active Search and Examination
- 2020-11-27 JP JP2022531386A patent/JP2023504250A/en active Pending
- 2020-11-27 LT LTEPPCT/EP2020/083787T patent/LT4064866T/en unknown
- 2020-11-27 BR BR112022010455A patent/BR112022010455A2/en unknown
- 2020-11-27 IL IL293172A patent/IL293172A/en unknown
- 2020-11-27 CN CN202080094839.XA patent/CN115243569A/en active Pending
- 2020-11-27 US US17/780,330 patent/US20230024853A1/en active Pending
- 2020-11-27 PL PL20816936.7T patent/PL4064866T3/en unknown
- 2020-11-27 EP EP20816936.7A patent/EP4064866B1/en active Active
- 2020-11-27 KR KR1020227017917A patent/KR20220122607A/en unknown
- 2020-11-27 CA CA3159870A patent/CA3159870A1/en active Pending
Non-Patent Citations (4)
Title |
---|
BRUCHET MARION ET AL: "Fabrication of patterned calcium cross-linked alginate hydrogel films and coatings through reductive cation exchange", CARBOHYDRATE POLYMERS, APPLIED SCIENCE PUBLISHERS , LTD BARKING, GB, vol. 131, 27 May 2015 (2015-05-27), pages 57 - 64, XP029252724, ISSN: 0144-8617, DOI: 10.1016/J.CARBPOL.2015.05.021 * |
GRANT G T ET AL: "Biological interactions between polysaccharides and divalent cations: The egg-box model", FEBS LETTERS, ELSEVIER, AMSTERDAM, NL, vol. 32, no. 1, 15 May 1973 (1973-05-15), pages 195 - 198, XP027202259, ISSN: 0014-5793, [retrieved on 19730515] * |
KUEN YONG LEE ET AL: "Alginate: Properties and biomedical applications", PROGRESS IN POLYMER SCIENCE, PERGAMON PRESS, OXFORD, GB, vol. 37, no. 1, 28 June 2011 (2011-06-28), pages 106 - 126, XP028334452, ISSN: 0079-6700, [retrieved on 20110705], DOI: 10.1016/J.PROGPOLYMSCI.2011.06.003 * |
SIKORSKI PAWEL ET AL: "Evidence for Egg-Box-Compatible Interactions in Calcium?Alginate Gels from Fiber X-ray Diffraction", BIOMACROMOLECULES, vol. 8, no. 7, 1 July 2007 (2007-07-01), US, pages 2098 - 2103, XP055837847, ISSN: 1525-7797, Retrieved from the Internet <URL:https://pubs.acs.org/doi/pdf/10.1021/bm0701503> DOI: 10.1021/bm0701503 * |
Also Published As
Publication number | Publication date |
---|---|
US20230024853A1 (en) | 2023-01-26 |
WO2021105465A1 (en) | 2021-06-03 |
AU2020391944A1 (en) | 2022-06-09 |
PL4064866T3 (en) | 2024-03-25 |
CA3159870A1 (en) | 2021-06-03 |
ES2969114T3 (en) | 2024-05-16 |
EP4064866A1 (en) | 2022-10-05 |
JP2023504250A (en) | 2023-02-02 |
GB201917472D0 (en) | 2020-01-15 |
LT4064866T (en) | 2024-02-12 |
BR112022010455A2 (en) | 2022-09-06 |
IL293172A (en) | 2022-07-01 |
PT4064866T (en) | 2024-01-24 |
CN115243569A (en) | 2022-10-25 |
KR20220122607A (en) | 2022-09-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US20230010782A1 (en) | Method of manufacturing an amorphous solid comprising an aerosol-former material | |
US20230087967A1 (en) | A consumable for use with a non-combustible aerosol provision system | |
US20230000135A1 (en) | Aerosol-generating comprising an amorphous solid with alginate and pectin as gelling agents | |
EP4064866B1 (en) | Aerosol-generating material comprising an amorphous solid comprising methol and calcium-crosslinked alginate | |
US20220408790A1 (en) | Method of making an amorphous solid for use with a non-combustible aerosol provision system | |
US20220408791A1 (en) | Aerosol generation | |
US20230018415A1 (en) | Aerosol generation | |
WO2021105437A1 (en) | Aerosol-generating material comprising an amorphous solid with carrageenan | |
EP4346456A1 (en) | Aerosol generating composition comprising nicotine and acid or nicotine salt | |
WO2023004092A1 (en) | Aerosol generating composition | |
AU2022314991A1 (en) | Aerosol generating composition | |
WO2023012303A1 (en) | Aerosol-generating material comprising chitosan and an additional binder | |
EP4380382A1 (en) | Aerosol-generating material comprising chitosan and an additional binder |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: UNKNOWN |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE |
|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
17P | Request for examination filed |
Effective date: 20220628 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
DAV | Request for validation of the european patent (deleted) | ||
DAX | Request for extension of the european patent (deleted) | ||
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R079 Ref document number: 602020023966 Country of ref document: DE Free format text: PREVIOUS MAIN CLASS: A24B0003140000 Ipc: A24B0015160000 Ref country code: DE Free format text: PREVIOUS MAIN CLASS: A24B0003140000 Ipc: A24B0015160000 |
|
P01 | Opt-out of the competence of the unified patent court (upc) registered |
Effective date: 20230505 |
|
RIC1 | Information provided on ipc code assigned before grant |
Ipc: A24C 5/01 20200101ALI20230526BHEP Ipc: A24B 15/16 20200101AFI20230526BHEP |
|
P02 | Opt-out of the competence of the unified patent court (upc) changed |
Effective date: 20230604 |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
INTG | Intention to grant announced |
Effective date: 20230803 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE PATENT HAS BEEN GRANTED |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 602020023966 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: SC4A Ref document number: 4064866 Country of ref document: PT Date of ref document: 20240124 Kind code of ref document: T Free format text: AVAILABILITY OF NATIONAL TRANSLATION Effective date: 20240119 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: GR Ref legal event code: EP Ref document number: 20240400274 Country of ref document: GR Effective date: 20240312 |
|
REG | Reference to a national code |
Ref country code: SK Ref legal event code: T3 Ref document number: E 43484 Country of ref document: SK |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: MP Effective date: 20240103 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2969114 Country of ref document: ES Kind code of ref document: T3 Effective date: 20240516 |