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United States Patent (19) 11 Patent Number: 5,927,288 Bensalem Et Al

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United States Patent (19) 11 Patent Number: 5,927,288 Bensalem Et Al USOO5927288A United States Patent (19) 11 Patent Number: 5,927,288 Bensalem et al. (45) Date of Patent: Jul. 27, 1999 54 HYDROMAGNESITE/MAGNESIUM 4,984,589 1/1991 Riedesser. HYDROXIDE FILLERS FOR SMOKING 5,121,759 6/1992 Dixit et al. .............................. 131/365 ARTICLE WRAPPERS AND METHODS FOR 55.8 CE E. - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 131/365 241 - 2 entry . MAKING SAME 5,228,463 7/1993 Fournier et al. ........................ 131/365 75 Inventors: AZZedline Bensalem, Brooklyn, N.Y.; FOREIGN PATENT DOCUMENTS Warren Chang, Taipei County, Taiwan; Jay A Fournier, Richmond, Va.; O404580 12/1990 European Pat. Off.. 544907 5/1942 United Kingdom. Andrew G. Kallianos, Asheville, N.C., 548.197 9/1942 United Kingdom. John B. Paine, III, Midlothian; 1289766 9/1972 United Kingdom. Kenneth F. Podraza, Richmond, both 2160084 12/1985 United Kingdom. of Va.; Donald M. Schleich, Carquefou, France; Jeffrey I. Seeman, Richmond, OTHER PUBLICATIONS Va. Menzel et al. Studien An Kohlensauren Magnesiumsalzen. I. 73 Assignee: Philip Morris Incorporated, New Basische Magnesiumcarbonate. Z. Electrochem. 1930. York, N.Y. Doelter et al. Weitere Vorläufige Mitteilungen über Arbeiten auf dem Grenzgebiete Zwischen Kolloidchemie, Mineralo 21 Appl. No.: 08/823,402 gie und Geologie. Z. Ch. Ind. Koll. 1909. L. Walter-Levy Contribution a letude de la double décom 22 Filed: Mar. 24, 1997 position entre les Solutions de Sulfate de magnésium et de carbonate de potassium, a l'bullition Séance du 1936. (51) Int. Cl. ................................................. A24D 1/02 L. Walter-Levy Carbonates basicques de magnésium. 52 U.S. Cl. .......................... 131/365; 131/358; 423/165; Acadénue Des Sciences 1935. 423/159; 423/430 Berak et al. Wplyw weglanu na Stopien dyspersi oraZ 58 Field of Search ..................................... 131/365, 358; Zachowanie termiczne Wytracanego Wodorotlenku magn 423/165, 159, 430; 162/8, 139 eZowego Przemysl Chemiczny 1960. 56) References Cited (List continued on next page.) U.S. PATENT DOCUMENTS Primary Examiner Mickey Yu 935,418 9/1909 Sisson ..................................... 423/165 Assistant Examiner Kelly O'Hara 1,361,324 12/1920 Grunwald ................................ 423/159 Attorney, Agent, or Firm-James T. Moore; James E. 1971,909 8/1934 Greider ................................... 423/430 Schardt, Charles E. B. Glenn 2,549,408 4/1951 Atchison. 2,673,565 3/1954 Schur et al.. 57 ABSTRACT 2,801,636 8/1957 Pfoh. 4,231,377 11/1980 Cline et al.. Hydromagnesite-magnesium hydroxide compositions are 4,420,002 12/1983 Cline. prepared which, when used as fillers in Smoking article 4,433,697 2/1984 Cline et al. ............................. 131/365 wrappers, Significantly reduce the amount of SideStream 4,450,847 5/1984 Owens .................................... 131/365 Smoke produced by the burning Smoking article while 4,561,454 12/1985 Guess. providing the Smoking article with good Subjective charac 4,805,644 2/1989 Hampl, Jr. et al.. teristics. 4,881,557 11/1989 Martin ..................................... 131/365 4.915,118 4/1990 Kaufman et al. ... 131/365 4.941,485 7/1990 Perfetti et al. .......................... 131/365 38 Claims, 10 Drawing Sheets HYDR MAGNESTE - 100,0 80,0 Z 60,0 40,0 2 10, O 2O,O 30,0 40, O 50, O 60,0 7O,O ANGE 5,927,288 Page 2 OTHER PUBLICATIONS McKie Subsolidus phase relations in the system Etude Sur les Carbonates de Magnésie: pp. 1021-1022; K.Ca(CO)-NaMg(CO) at 1 kbar: The fairchildite 1065-1069; 1114–1118 La Papeterie 1920. buetschlite-eitelite eutectoid American Mineralogist 1990. Brausser A Propos Des Propriétés De L'Eitelite Deelman Low-temperature Synthesis of eitelite, NaMg(CO). Bulletin de la Société Royale 1967. NaCOMgCO. N. Jb. Miner. Mn. 1984. Frankis et al. Subsolidus Relations in the System NaCO Pabst The Cystallography and Structure of Eitelite, CaCo-HO Nature Physical Science 1973. NaMg(CO) American Mineralogist 1955. U.S. Patent Jul. 27, 1999 Sheet 1 of 10 5,927.288 5.5. OO Q. s i. M SST HOIM U.S. Patent Jul. 27, 1999 Sheet 2 of 10 5,927.288 CO vm C were Y O 8 in e Cd CU CO SP L Y O Has C Y Co LL r Ll H O CU C O - A V?) O NO g G?NIW / SSOT HOIGM. A. U.S. Patent Jul. 27, 1999 Sheet 3 of 10 5,927.288 S. 3.5. U.S. Patent Jul. 27, 1999 Sheet 4 of 10 5,927.288 5. % 74 SSO HOIGW U.S. Patent Jul. 27, 1999 Sheet S of 10 5,927.288 Cs Q C H 0 OO ornu re C Cl OO r SP Y D H < Y Co LL (J - r > L He O Cl (U O H r Cy) w(U G?NIW / A, SSD HEDIW U.S. Patent Jul. 27, 1999 Sheet 6 of 10 5,927.288 O O Q O ve OD o r O C OO R. S. L Y D - < C) - (J - w > l H l O CU C co OO V O S Cl U.S. Patent Jul. 27, 1999 Sheet 7 of 10 5,927.288 O OOT 06 08 OZ O9 OC O7 O8 Oe O O s --------------------- s 5. 5. 5 5 s S S d cd OLT OOT O6 O8 OA, O9 OC O7 O8 Oct. O O C 4 SSWW U.S. Patent Jul. 27, 1999 Sheet 8 of 10 5,927.288 s : s 5. 5. f s MISNNI U.S. Patent Jul. 27, 1999 Sheet 9 of 10 5,927.288 s ; WISN.INI U.S. Patent Jul. 27, 1999 Sheet 10 0f 10 5,927.288 s ; AISN.INI 5,927,288 1 2 HYDROMAGNESITE/MAGNESIUM of temperature, preSSure, and concentration of materials, HYDROXIDE FILLERS FOR SMOKING heterogeneous reaction conditions, which impact the forma ARTICLE WRAPPERS AND METHODS FOR tion and location of nucleation sites and crystallization MAKING SAME characteristics, and the like. Many references detail the production of Synthetic basic I. BACKGROUND magnesium carbonate (hydromagnesite Mg(CO) (OH)2.4H2O), including U.S. Pat. Nos. 1971,909, 1,361, A. Field of the Invention 324, 935,418; British Pat. Nos. 548,197 and 544,907; See The present invention relates to novel fillers for Smoking also Z. KSt., 1910, 47, 118 and Z. Ch. Ind. Koll. 1909, 4, article wrappers, and to processes for making them. 189.) In these cases, aqueous Solutions of magnesium bicar B. Description of the Prior Art bonate Mg(HCO) were formed, typically incorporating a carbonation Step, and then transformed by the action of base, SideStream Smoke is the Smoke given off by the burning e.g., magnesium hydroxide, to form basic magnesium car end of a cigarette or a cigarette-like Smoking article between bonate. However, none of these attempts attempted, puffs. Such Smoke may be objectionable to Some near the reported, or asserted the formation of compositions contain Smoker who are not Smoking or who do not Smoke. 15 ing both hydromagnesite and magnesium hydroxide. In Therefore, cigarettes that produce leSS SideStream Smoke are addition, none of these attempts Specified examining various highly desirable. reaction conditions and varying molar ratioS of carbon Several attempts have been made to reduce SideStream dioxide and other Starting materials to form Specific com Smoke through the use of various compounds as fillers for positions containing both hydromagnesite and magnesium Smoking article wrappers. For example, magnesium hydrox hydroxide. In addition, none of these attempts described any ide and magnesium oxide have been reported to reduce effort to modify morphology and obtain material sharing SideStream Smoke in cigarettes, as disclosed in U.S. Pat. Specific particle sizes and agglomerate sizes. Nos. 5,131416, 4,941,485, 4,915,118, 4,881,557, 4,433, Nesquehonite (MgCO.3H2O) was formed by passing a 697, and 4,231,377. Some smokers find that cigarettes made 2-3%. Solution of magnesium bicarbonate through a Series of with wrapperS containing these compounds have an unac 25 tanks at about 38°C. while magnesium oxide was added to ceptably poor taste. the last tank, as disclosed in U.S. Pat. No. 2,549,408. Others have tried colloidal Solutions of magnesium Hydromagnesite and magnesium hydroxide were hydroxide, e.g. as disclosed by U.S. Pat. No. 4,450,847. obtained in the reaction of a Soluble magnesium Salt at Again, while magnesium hydroxide reduces the amount of relatively low temperatures by exceSS potassium carbonate SideStream Smoke, its incorporation into Smoking article or by potassium carbonate/potassium hydroxide. In this wrappers often results in a cigarette with unacceptably poor case, the initially formed precipitate is amorphous and later taSte. becomes crystalline, as described in H. Menzel and A. Some have used physical mixtures of magnesium hydrox Brueckner, Z. Electrochem., 1930, 36, 63–87. If a ide or an unspecified "magnesium carbonate' composition magnesium-potassium mixed carbonate is used in the with other compounds Such as calcium carbonate in Smoking 35 reaction, the products contain phases having both magne article wrappers without Solving the poor taste problem, as sium and potassium. (See L. Walter-Levy, Compt. rend. in U.S. Pat. No. 4,984,589. 1935, 200, 1940–1942.) Various grades of commercial basic magnesium In another case, basic magnesium carbonate is treated carbonate, the Standard industrial name for hydromagnesite, with Sodium hydroxide to yield pure magnesium hydroxide. Mg(CO)(OH)(4HO), have been disclosed as the inor 40 (See Brit. Pat. No. 547,769.) The double decomposition of ganic filler in cigarette papers to produce cigarettes having Solutions of magnesium Sulfate and potassium carbonate at reduced SideStream Smoke. One Such example is U.S. Pat. the boiling point result in the formation of various double No. 5,121,759. However, there is no teaching or suggestion carbonates.
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