US3760815A - Preparation of reconstituted tobacco - Google Patents
Preparation of reconstituted tobacco Download PDFInfo
- Publication number
- US3760815A US3760815A US00104459A US3760815DA US3760815A US 3760815 A US3760815 A US 3760815A US 00104459 A US00104459 A US 00104459A US 3760815D A US3760815D A US 3760815DA US 3760815 A US3760815 A US 3760815A
- Authority
- US
- United States
- Prior art keywords
- tobacco
- acids
- acid
- slurry
- ammonium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 62
- 241000208125 Nicotiana Species 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title description 2
- 239000001814 pectin Substances 0.000 claims abstract description 24
- 229920001277 pectin Polymers 0.000 claims abstract description 24
- 235000010987 pectin Nutrition 0.000 claims abstract description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 22
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 15
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011575 calcium Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 36
- 239000002253 acid Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 29
- 150000007513 acids Chemical class 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 8
- 235000021313 oleic acid Nutrition 0.000 claims description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- -1 magnesium carboxylates Chemical class 0.000 claims description 6
- 230000000391 smoking effect Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 150000007519 polyprotic acids Polymers 0.000 claims description 3
- 239000001195 (9Z,12Z,15Z)-octadeca-9,12,15-trienoic acid Substances 0.000 claims description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid ester group Chemical group C(CCCCCCCCCCC)(=O)O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical group [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 abstract description 9
- 235000005985 organic acids Nutrition 0.000 abstract description 7
- 235000019505 tobacco product Nutrition 0.000 abstract description 7
- 239000011230 binding agent Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 159000000003 magnesium salts Chemical class 0.000 abstract description 4
- 150000002891 organic anions Chemical class 0.000 abstract description 2
- 238000005266 casting Methods 0.000 description 13
- 239000000428 dust Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 229910001868 water Inorganic materials 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 235000019504 cigarettes Nutrition 0.000 description 6
- 239000000779 smoke Substances 0.000 description 6
- 229920002230 Pectic acid Polymers 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 235000015165 citric acid Nutrition 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 235000020778 linoleic acid Nutrition 0.000 description 2
- OYHQOLUKZRVURQ-HZJYTTRNSA-N linoleic acid group Chemical group C(CCCCCCC\C=C/C\C=C/CCCCC)(=O)O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 2
- 125000005481 linolenic acid group Chemical group 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 244000061176 Nicotiana tabacum Species 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
- FVFJGQJXAWCHIE-UHFFFAOYSA-N [4-(bromomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CBr)C=C1 FVFJGQJXAWCHIE-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 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
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- SATJMZAWJRWBRX-UHFFFAOYSA-N azane;decanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCCCCCC([O-])=O SATJMZAWJRWBRX-UHFFFAOYSA-N 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical class [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 235000011160 magnesium carbonates Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 239000010318 polygalacturonic acid Substances 0.000 description 1
- YQUVCSBJEUQKSH-UHFFFAOYSA-N protochatechuic acid Natural products OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000007761 roller coating Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000008371 vanilla flavor Substances 0.000 description 1
- WKOLLVMJNQIZCI-UHFFFAOYSA-N vanillic acid Chemical compound COC1=CC(C(O)=O)=CC=C1O WKOLLVMJNQIZCI-UHFFFAOYSA-N 0.000 description 1
- TUUBOHWZSQXCSW-UHFFFAOYSA-N vanillic acid Natural products COC1=CC(O)=CC(C(O)=O)=C1 TUUBOHWZSQXCSW-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/12—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
Definitions
- the patents describe the release of pectins and pectinic substances from the tobacco parts for subsequent redeposit on the same or other tobacco parts as adhesives to bind them into a coherent sheet or other form.
- the pectin release is carried out by the use of special agents which act by removing the divalent metal cross-links, essentially calcium and magnesium by a number of methods, for example, a method utilizing additive substances which remove the divalent metal ions by forming relatively insoluble salts; a method which removes the ions by an additive causing a chelating or sequestering action; or by another method which acidifies the system with an acid and produces soluble salts of Ca and Mg, which can be washed out, leaving the pectins in the insoluble acid form, but which then requires an alkalinizing step to solubilize the pectins.
- ashforming ingredients may increase the delivery of total particulate matter (TPM) in the smoke.
- TPM total particulate matter
- the present invention is an improvement in the production of a reconstituted tobacco in that the release of tobacco pectins in situ may be accomplished without the addition of ash-forming inorganic salts or acids, while at the same time, enhancing the flavor and aroma of the smoke. 1
- selected monobasic organic acids of six to 18 carbon atoms or polybasic acids of two to 12 carbon atoms and ammonium hydroxide or ammonium salts of such acids are added to tobacco parts as cross-links destroying agents.
- the latter additives or components thereof are volatilized in subsequent drying operations, or are burned in smoking to produce principally the same products that arise from combustion of tobacco without additives, namely, carbon dioxide, water, ammonia, and the like, so that ash appearance and, more importantly, TPM delivery are substantially unchanged.
- Smoking of the products has shown the flavor to be acceptable, and sometimes enhanced and novel, mild rather than harsh, with no undesirable foreign notes.
- the sheet produced is pliable and plastic, and added plasticizer (e.g., triethylene glycol) may be reduced or eliminated.
- the process comprises the treatment of the tobacco parts, preferably in finely divided form, with an aqueous solution or suspension of selected organic acids with ammonium hydroxide or the ammonium salt of one or more of these acids, in the presence of excess ammonium hydroxide.
- the treatment of the tobacco in the presence of these ammonium salts and ammonium hydroxide results in the release of the pectinaceous components from the tobacco in the form of ammonium pectates.
- the original pectinaceous components with may be termed protopectins, consist essentially of calcium and/or magnesium salts of polygalacturonic acid, the divalent metallic atoms acting as cross-links between the galacturonic chains, these being destroyed in the reaction.
- the calcium and/or magnesium cations form substantially water-insoluble salts with the anionic groups, particularly when the pH is in the alkaline range.
- These insoluble salts, together with the ammonium pectates acting as binding agents, are combined with the treated tobacco and are extruded, cast or otherwise formed into a reconstituted tobacco product which may then be processed in known manner to produce the desired form of smoking product.
- the organic acids that are selected are unsubstituted aliphatic or aromatic mono or polycarboxylic acids or such acids having only hydroxy and lower alkoxy groups as substituents.
- the acids should consist only of carbon, hydrogen and oxygen.
- the monocarboxylic acids preferred are fatty acids having six to 18 carbon atoms while the preferred polycarboxylic acids are those having two to 12 carbon atoms.
- These acids should have the general characteristic of forming calcium or magnesium salts that, under the conditions of treatment, particularly in an alkaline environment well above pH 8, preferably pH 9 to 10, are substantially insoluble in the aqueous medium.
- these salts either volatilize off, or alternatively, break down during the combustion of the tobacco to calcium or magnesium carbonates, carbon dioxide, water and, in fact, the same elements normally released when untreated tobacco is burned.
- ammonium components eitheras ammonium pectates or substantially trace amounts of free ammonia or ammonium hydroxide, ammonia gas is volatilized out either before the product is smoked, that is during the drying step, or certainly during the combustion. The end result is that the combustion of the treated tobacco produces the same type of ash as would be produced from the combusion of tobacco that had not been treated and was free of additives.
- citric, malic or vanillic acids or other flavor or aroma inducing acids with ammonium hydroxide, or alternatively their ammonium salts, with excess ammonia, when used for the release of pectins and waterinsoluble salts, will also produce an exceptionally flavorful smoke.
- the longer-chain fatty acids either saturated or unsaturated, for example, stearic, oleic, linoleic or linolenic acids or their ammonium salts, these provide not only a subtle flavor characteristic of the smoke when used in the desired concentration, but also possess a plasticizing effect that requires little or no added plasticizers normally used in making a reconstituted tobacco product.
- the preferred acids that may be used in carrying out the process of the invention are citric, malic, gluconic, oxalic, tartaric, mellitic, vanillic, sebacic, lauric, stearic, oleic, linoleic or linolenic acids.
- Particularly preferred acids are citric or malic acids. As indicated previously, one may use a single acid or a mixture of different acids.
- tobacco plant parts usually waste or scrap tobacco parts in the form of flakes, shreds, tobacco fines or dust, but preferably in finely divided form, is slurried with an aqueous solution of an ammonium salt ofa selected organic acid or a mixture of such salts.
- the amount of added salt may be in the range of about 0.0 to about 0.25 mols of salt per 100 grams of tobacco, but preferably in an amount of about 0.025 to 0.08 mols per 100 grams of tobacco.
- sufficient ammonium hydroxide must be added to reach an alkaline pH, preferably from pH 9 to about pH 10.
- the slurry is maintained at a temperature of from about 25 to 110C. for about one-half to 24 hours. Heating may not be necessary since heat may be generated by the reaction taking place in the treating vessel. While heating or cooking is being carried out, more ammonia may be needed to maintain the alkaline pH. After sufficient time has elapsed and when the reaction is substantially completed, the tobacco slurry may be refined by use ofa rapid or high speed beater, followed by deaeration before casting, spraying, roller-coating or the like in reconstituted tobacco forms such as webs, sheets, fibers or other desired forms.
- ammonium salts instead of using ammonium salts as such, one may form these salts in situ or at least have the desired anions and cations present by using one or more organic acids and sufficient ammonium hydroxide, usually in excess so as to result in an alkaline pH of pH 9 or higher.
- Sufficient ammonium hydroxide is then added to result in the slurry achieving an alkaline pH in the range of 9 to l0.
- ammonium pectins would be formed from the re leased pectins and the calcium and magnesium cross linking cations of the tobacco protopectins would form salts with the acidic anions.
- the entire reaction mix may then be cast, extruded, sprayed or otherwise treated to solidify the solids by procedures well known in the art, to form a reconstituted tobacco product.
- Example 1 A slurry was prepared in a Waring blender from 50 g of tobacco dust (-50 mesh), 450 ml. of water, 1.0 g of citric acid, and sufficient aqueous ammonia to raise the pH to 9.5. The slurry was refined by beating for 30 minutes, at which time the temperature had reached C. The viscosity had reached a maximum after five minutes. No additional heat was applied. The slurry was deaerated under vacuum on a steam bath (pH after cooling, 8.8). The hot slurry was cast on steel plates by using a casting knife set at 50 mils, dried over a steam bath, and stripped from the plates. A uniform, dense sheet without pinholes resulted. Its properties were:
- Example 2 Portions of tobacco dust (50 mesh) and water, 50 g and 450 ml. respectively, were treated with additives and conditions as listed in Table I, using a Waring blender for refining and a steam bath for heating. Deaeration after refining was for 10 minutes except the last run where 1 hr. heating took its place. Casting on steel plates with a casting knife set at 50 mils, and drying produced sheets with the properties listed in Table Example 3 Tobacco dust (50 g, 50 mesh) and citric acid (7.5 g) were slurried with 285 ml. water in a Waring blender. To the slurry concentrated NH OH was added to pH 9.0 which was maintained during the heating period.
- the slurry was heated to C in a steam bath for 2 hours, and refined for 1 minute.
- the hot slurry was cast on steel plates using a casting knife set at 35 mils, dried over a steam bath and doctored off. pH of the cold slurry was 8.7, sheet pH was 5.3. The sheet was satisfactory but it did have many fine cracks.
- Example 4 A slurry consisting of 1,019.4 lb. water, 174.8 lb. tobacco dust, 24.6 lb. citric acid, and 42 lb. of 30% NH OH was prepared in a mixing tank. The temperature was maintained Not decorated before casting.
- the sheets were cut into filler and cigarettes were prepared for smoke test comparison against a standard cigarette, as shown in Table 11 below.
- mm. filter tips were attached to the cigarettes, and then 50 mm. of cigarettes smoked for TPM and nicotine.
- Example 5 Sebacic acid (5 g), 50 g tobacco dust (-50 mesh), and 450 ml. H O were slurried in a Waring blender. Concentrated NH OH was added to raise pH to 9.5. The slurry was refined for 30 minutes during which period the temperature was raised to 90 C. After the refining, the slurry was heated on a steam bath in order to deaerate. It was then cast on stainless steel plates using a casting knife with 50 mils setting. To dry the product the plates were placed over a steam bath. The sheets were doctored.
- Example 6 Mellitic acid (5 g), 50 g tobacco dust (-50 mesh), and 450 m1. H O were slurried in a Waring blender.
- Example 7 Ten grams oleic acid, 50 g tobacco dust, and 450 ml. H O were slurried in a Waring blender. pH was adjusted to 9.0 with concentrated NH OH. The slurry was heated at 90 C. over a steam bath for 1 hour, re-
- the slurry was heated oon a steam bath for one hour
- slurry was cast on stainless steel plates using a casting knife set at 50 mils, dried over a steam bath and doctored.
- the product was soft and plastic.
- Ammonium oleate (10.6 g) may be used in place of the oleic acid in the above example, and using sufficient ammonium hydroxide to obtain a pH of 9.
- the heating, refining and casting are described above.
- the product is the equivalent of that given in the example.
- Example 8 Vanillic acid (8.4 g), 50 g tobacco dust and 450 ml, H O were slurried in a Waring blender. pH was adjusted to 9.3 with concentrated NH OH. The slurry was heated for 2 hours at C. in a steam bath, refined for 10 minutes, and deaerated for 15 minutes. The slurry was cast on stainless steel plates using a casting knife set at 50 mils, dried over a steam bath and doctored. The product had a subtle sweet aroma. Cigarettes prepared from this product when smoked had a subtle vanilla flavor both in the main and side streams.
- Example 9 Ammonium sebacate (6 g) and 50 g (-50 mesh) of tobacco dust were slurried in 450 ml. H O in a Waring blender. The pH was adjusted to pH 9.0 with concentrated NH OH. The slurry was brought to 90 C. and held at that temperature for 1 hour. It was refined for 30 minutes and then heated on a steam bath to deaerate for about 30 minutes. The slurry was cast on stainless steel plates using a casting knife set at 50 mils, then dried over a steam bath and doctored. The product had similar characteristics to the product of Example 5.
- Example 10 Eighty pounds of tobacco dust having a pH of 5.7, 12 lb. 8 oz. concentrated NH OH, and 454 lb. H O were placed in a vat with steam coils and circulating pump. The slurry was heated to about 90 C. for one hour while being constantly circulated during the heating. The slurry was recycled through refiners for about 45 minutes. The temperature was maintained at about 90 C. and additional Nl-LOH was added to maintain pH at 9.0. When refining was completed the total solids were 17 percent and the viscosity approximately 8,000 centipoises at 2% RPM, spindle D, using Brookfield wire T- form spindle. A portion of the slurry after deaeration was hand cast on stainless steel plates at 50 mils, using a casting knife.
- step (a) is in finely divided form.
- said reagent comprises a polycarboxylic acid of two to 12 carbon atoms and ammonium hydroxide.
- said reagent comprises a monocarboxylic fatty acid having six to 18 carbon atom and ammonium hydroxide.
- reaction is carried out in the presence of ammonium cations and organic acid anions derived from acids of the group consisting of oxalic, citric, malic, sebacic, tartaric, mellitic, vanillic, gluconic, stearic, lauric, oleic, linoleic and linolenic acids.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
- Paper (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10445971A | 1971-01-06 | 1971-01-06 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3760815A true US3760815A (en) | 1973-09-25 |
Family
ID=22300591
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00104459A Expired - Lifetime US3760815A (en) | 1971-01-06 | 1971-01-06 | Preparation of reconstituted tobacco |
Country Status (7)
Country | Link |
---|---|
US (1) | US3760815A (enrdf_load_stackoverflow) |
CA (1) | CA958959A (enrdf_load_stackoverflow) |
CH (1) | CH565518A5 (enrdf_load_stackoverflow) |
DE (2) | DE2200488C3 (enrdf_load_stackoverflow) |
FR (1) | FR2120990A5 (enrdf_load_stackoverflow) |
GB (1) | GB1321179A (enrdf_load_stackoverflow) |
NL (1) | NL7200124A (enrdf_load_stackoverflow) |
Cited By (56)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4286606A (en) * | 1979-06-18 | 1981-09-01 | Philip Morris Incorporated | Tobacco flavorants |
US4607646A (en) * | 1984-02-06 | 1986-08-26 | Philip Morris Incorporated | Process for modifying the smoke flavor characteristics of tobacco |
US4625737A (en) * | 1982-12-30 | 1986-12-02 | Philip Morris Incorporated | Foamed, extruded, tobacco-containing smoking article and method of making the same |
US4632131A (en) * | 1984-07-03 | 1986-12-30 | Philip Morris Incorporated | Foamed, extruded, coherent multistrand smoking articles |
US4674519A (en) * | 1984-05-25 | 1987-06-23 | Philip Morris Incorporated | Cohesive tobacco composition |
DE3705879A1 (de) * | 1986-02-24 | 1987-08-27 | Brown & Williamson Tobacco | Verbessertes verfahren zum behandeln, trocknen und expandieren von tabak |
GB2210547A (en) * | 1987-10-05 | 1989-06-14 | Brown & Williamson Tobacco | Forming flavour compounds in tobacco |
US4874000A (en) * | 1982-12-30 | 1989-10-17 | Philip Morris Incorporated | Method and apparatus for drying and cooling extruded tobacco-containing material |
US5099864A (en) * | 1990-01-05 | 1992-03-31 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
US5129409A (en) * | 1989-06-29 | 1992-07-14 | R. J. Reynolds Tobacco Company | Extruded cigarette |
US5325877A (en) * | 1993-07-23 | 1994-07-05 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
US5327917A (en) * | 1990-08-15 | 1994-07-12 | R. J. Reynolds Tobacco Company | Method for providing a reconstituted tobacco material |
US5339838A (en) * | 1992-08-17 | 1994-08-23 | R. J. Reynolds Tobacco Company | Method for providing a reconstituted tobacco material |
US5377698A (en) * | 1993-04-30 | 1995-01-03 | Brown & Williamson Tobacco Corporation | Reconstituted tobacco product |
US5533530A (en) * | 1994-09-01 | 1996-07-09 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
US5727571A (en) * | 1992-03-25 | 1998-03-17 | R.J. Reynolds Tobacco Co. | Components for smoking articles and process for making same |
WO1999029190A1 (en) * | 1997-12-08 | 1999-06-17 | Brown & Williamson Tobacco Corporation | A method for making a reconstituted tobacco sheet using steam exploded tobacco |
WO1999029189A1 (en) * | 1997-12-08 | 1999-06-17 | Brown & Williamson Tobacco Corp. | A method for making a reconstituted tobacco sheet using steam exploded tobacco |
US6440223B1 (en) | 2000-02-15 | 2002-08-27 | R. J. Reynolds Tobacco Co. | Smoking article containing heat activatable flavorant-generating material |
US6499489B1 (en) | 2000-05-12 | 2002-12-31 | R. J. Reynolds Tobacco Company | Tobacco-based cooked casing formulation |
US6679270B2 (en) | 2000-10-05 | 2004-01-20 | Nicolas Baskevitch | Reduction of nitrosamines in tobacco and tobacco products |
US6695924B1 (en) | 2000-07-25 | 2004-02-24 | Michael Francis Dube | Method of improving flavor in smoking article |
US20040173228A1 (en) * | 2003-03-04 | 2004-09-09 | R. J. Reynolds Tobacco Company | Method for producing flavorful and aromatic compounds from tobacco |
US20040255965A1 (en) * | 2003-06-17 | 2004-12-23 | R. J. Reynolds Tobacco Company | Reconstituted tobaccos containing additive materials |
US20050005947A1 (en) * | 2003-07-11 | 2005-01-13 | Schweitzer-Mauduit International, Inc. | Smoking articles having reduced carbon monoxide delivery |
US20050263161A1 (en) * | 2004-05-27 | 2005-12-01 | Brown & Williamson Tobacco Corporation | Tobacco filler of low nitrogen content |
US20060162733A1 (en) * | 2004-12-01 | 2006-07-27 | Philip Morris Usa Inc. | Process of reducing generation of benzo[a]pyrene during smoking |
US20060174904A1 (en) * | 2005-02-07 | 2006-08-10 | Schweitzer-Mauduit International, Inc. | Smoking articles having reduced analyte levels and process for making same |
US20070295348A1 (en) * | 2006-06-01 | 2007-12-27 | Schweitzer-Mauduit International, Inc. | Free air burning smoking articles with reduced ignition proclivity characteristics |
US20080178894A1 (en) * | 2007-01-26 | 2008-07-31 | Philip Morris Usa Inc. | Methods and apparatus for the selective removal of constituents from aqueous tobacco extracts |
US20090025738A1 (en) * | 2007-07-23 | 2009-01-29 | R. J. Reynolds Tobacco Company | Smokeless Tobacco Composition |
US20090025739A1 (en) * | 2007-07-23 | 2009-01-29 | R. J. Reynolds Tobacco Company | Smokeless Tobacco Composition |
US20100037903A1 (en) * | 2008-08-14 | 2010-02-18 | R. J. Reynolds Tobacco Company | Method for Preparing Flavorful and Aromatic Compounds |
EP2179666A2 (en) | 2007-07-23 | 2010-04-28 | R.J.Reynolds Tobacco Company | Smokeless Tobacco Compositions And Methods For Treating Tobacco For Use Therein |
US20100300463A1 (en) * | 2009-06-02 | 2010-12-02 | R.J. Reynolds Tobacco Company | Thermal treatment process for tobacco materials |
US20110048434A1 (en) * | 2009-06-02 | 2011-03-03 | R. J. Reynolds Tobacco Company | Thermal treatment process for tobacco materials |
WO2011081725A1 (en) | 2009-12-15 | 2011-07-07 | R. J. Reynolds Tobacco Company | Tobacco product and method for manufacture |
WO2012170761A1 (en) | 2011-06-10 | 2012-12-13 | Schweitzer-Mauduit International, Inc. | Tobacco material containing non-isometric calcium carbonate microparticles |
WO2013074903A1 (en) | 2011-11-18 | 2013-05-23 | R. J. Reynolds Tobacco Company | Smokeless tobacco product comprising tobacco - derived pectin component |
WO2013170028A1 (en) | 2012-05-09 | 2013-11-14 | Lanig Le Bec | Tobacco product that produces lower carbon monoxide to tar ratio |
WO2014134254A1 (en) | 2013-02-28 | 2014-09-04 | Schweitzer-Mauduit International, Inc. | Composition for making a tea beverage or herbal and vegetable broths |
WO2014141201A2 (en) | 2013-03-15 | 2014-09-18 | Fall Safall | Method of reducing tobacco-specific nitrosamines |
WO2014140346A1 (en) | 2013-03-15 | 2014-09-18 | Philip Morris Products S.A | Methods for reducing one or more tobacco specific nitrosamines in tobacco material |
WO2014207704A2 (en) | 2013-06-26 | 2014-12-31 | Pan Jiayi | Filter media |
US8991403B2 (en) | 2009-06-02 | 2015-03-31 | R.J. Reynolds Tobacco Company | Thermal treatment process for tobacco materials |
US9149068B2 (en) | 2012-10-11 | 2015-10-06 | Schweitzer-Mauduit International, Inc. | Wrapper having reduced ignition proclivity characteristics |
CN109077347A (zh) * | 2018-07-20 | 2018-12-25 | 河南卷烟工业烟草薄片有限公司 | 一种提高造纸法再造烟叶中有机氮的涂布剂、其制备方法及应用 |
US10178872B2 (en) | 2010-10-29 | 2019-01-15 | Schweitzer-Manduit International, Inc. | Method for producing articles of plant origin impregnated with a liquid plant substance |
EP3561179A1 (en) | 2014-03-28 | 2019-10-30 | SWM Luxembourg s.a.r.l. | Reconstituted plant material and its use for packaging, wrapping and food appliances |
US10729662B2 (en) | 2013-08-20 | 2020-08-04 | Schweitzer-Mauduit International, Inc. | Product comprising a plant for medicinal, cosmetic, coloring or dermatologic use |
US10751282B2 (en) | 2013-08-02 | 2020-08-25 | Schweitzer-Mauduit International, Inc. | Edible product comprising reconstituted plant material |
US11035079B2 (en) | 2016-04-05 | 2021-06-15 | Schweitzer-Mauduit International, Inc. | Vegetable paper comprising fibres of a plant |
CN114698867A (zh) * | 2022-04-08 | 2022-07-05 | 贵州黄果树金叶科技有限公司 | 一种精准成分再造烟叶制备方法及再造烟叶 |
US11484497B2 (en) | 2013-02-28 | 2022-11-01 | Schweitzer-Mauduit International, Inc. | Composition for making a tea beverage or herbal and vegetable broths |
US11737472B2 (en) | 2015-03-02 | 2023-08-29 | Mativ Holdings, Inc. | Low bulk density composition for making a tea beverage having reduced dust or fines |
US12201142B2 (en) | 2020-09-11 | 2025-01-21 | SWM Holdings US, LLC | Filter for smoking or vaping article comprising a nonwoven substrate |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0162671B1 (en) * | 1984-05-25 | 1991-08-21 | Philip Morris Products Inc. | Cohesive tobacco composition |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US3306307A (en) * | 1964-04-17 | 1967-02-28 | American Mach & Foundry | Treatment of tobacco |
US3420241A (en) * | 1967-04-28 | 1969-01-07 | Philip Morris Inc | Method of preparing a reconstituted tobacco sheet employing a pectin adhesive |
CH480029A (de) * | 1963-09-02 | 1969-10-31 | Tamag Basel Ag | Verfahren zur Herstellung von Tabakfolien |
-
1971
- 1971-01-06 US US00104459A patent/US3760815A/en not_active Expired - Lifetime
- 1971-12-07 CA CA129,533A patent/CA958959A/en not_active Expired
- 1971-12-17 GB GB5866071A patent/GB1321179A/en not_active Expired
- 1971-12-28 FR FR7147050A patent/FR2120990A5/fr not_active Expired
-
1972
- 1972-01-05 DE DE2200488A patent/DE2200488C3/de not_active Expired
- 1972-01-05 DE DE19722265372 patent/DE2265372A1/de not_active Withdrawn
- 1972-01-05 NL NL7200124A patent/NL7200124A/xx unknown
- 1972-01-06 CH CH18272A patent/CH565518A5/xx not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CH480029A (de) * | 1963-09-02 | 1969-10-31 | Tamag Basel Ag | Verfahren zur Herstellung von Tabakfolien |
US3306307A (en) * | 1964-04-17 | 1967-02-28 | American Mach & Foundry | Treatment of tobacco |
US3420241A (en) * | 1967-04-28 | 1969-01-07 | Philip Morris Inc | Method of preparing a reconstituted tobacco sheet employing a pectin adhesive |
Cited By (86)
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US4286606A (en) * | 1979-06-18 | 1981-09-01 | Philip Morris Incorporated | Tobacco flavorants |
US4874000A (en) * | 1982-12-30 | 1989-10-17 | Philip Morris Incorporated | Method and apparatus for drying and cooling extruded tobacco-containing material |
US4625737A (en) * | 1982-12-30 | 1986-12-02 | Philip Morris Incorporated | Foamed, extruded, tobacco-containing smoking article and method of making the same |
US4607646A (en) * | 1984-02-06 | 1986-08-26 | Philip Morris Incorporated | Process for modifying the smoke flavor characteristics of tobacco |
US4674519A (en) * | 1984-05-25 | 1987-06-23 | Philip Morris Incorporated | Cohesive tobacco composition |
US4632131A (en) * | 1984-07-03 | 1986-12-30 | Philip Morris Incorporated | Foamed, extruded, coherent multistrand smoking articles |
DE3705879A1 (de) * | 1986-02-24 | 1987-08-27 | Brown & Williamson Tobacco | Verbessertes verfahren zum behandeln, trocknen und expandieren von tabak |
AU592716B2 (en) * | 1987-10-05 | 1990-01-18 | Brown & Williamson Tobacco Corporation | Process for forming flavour compounds in tobacco |
GB2210547A (en) * | 1987-10-05 | 1989-06-14 | Brown & Williamson Tobacco | Forming flavour compounds in tobacco |
GB2210547B (en) * | 1987-10-05 | 1991-07-03 | Brown & Williamson Tobacco | Process for forming flavour compounds in tobacco. |
US5129409A (en) * | 1989-06-29 | 1992-07-14 | R. J. Reynolds Tobacco Company | Extruded cigarette |
US5099864A (en) * | 1990-01-05 | 1992-03-31 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
US5327917A (en) * | 1990-08-15 | 1994-07-12 | R. J. Reynolds Tobacco Company | Method for providing a reconstituted tobacco material |
US5727571A (en) * | 1992-03-25 | 1998-03-17 | R.J. Reynolds Tobacco Co. | Components for smoking articles and process for making same |
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US5377698A (en) * | 1993-04-30 | 1995-01-03 | Brown & Williamson Tobacco Corporation | Reconstituted tobacco product |
US5325877A (en) * | 1993-07-23 | 1994-07-05 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
US5533530A (en) * | 1994-09-01 | 1996-07-09 | R. J. Reynolds Tobacco Company | Tobacco reconstitution process |
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US20040173228A1 (en) * | 2003-03-04 | 2004-09-09 | R. J. Reynolds Tobacco Company | Method for producing flavorful and aromatic compounds from tobacco |
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US12201142B2 (en) | 2020-09-11 | 2025-01-21 | SWM Holdings US, LLC | Filter for smoking or vaping article comprising a nonwoven substrate |
CN114698867B (zh) * | 2022-04-08 | 2023-03-03 | 贵州黄果树金叶科技有限公司 | 一种精准成分再造烟叶制备方法及再造烟叶 |
CN114698867A (zh) * | 2022-04-08 | 2022-07-05 | 贵州黄果树金叶科技有限公司 | 一种精准成分再造烟叶制备方法及再造烟叶 |
Also Published As
Publication number | Publication date |
---|---|
CA958959A (en) | 1974-12-10 |
NL7200124A (enrdf_load_stackoverflow) | 1972-07-10 |
DE2200488A1 (de) | 1972-07-20 |
DE2200488B2 (de) | 1978-01-05 |
DE2265372A1 (de) | 1977-10-13 |
GB1321179A (en) | 1973-06-20 |
FR2120990A5 (enrdf_load_stackoverflow) | 1972-08-18 |
AU3659671A (en) | 1973-06-14 |
CH565518A5 (enrdf_load_stackoverflow) | 1975-08-29 |
DE2200488C3 (de) | 1978-09-14 |
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