US2977254A - Smoking product - Google Patents

Description

United States Patent SMOKING PRODUCT Sheldon Rosenberg, Westport, and Otto Karl Schmidt, Springdale, Conn., assignors to International Cigar Machinery Company, Inc., a corporation of New Jersey No Drawing. Filed Sept. 9, 1959, Ser. No. 838,854

11 Claims. (Cl. 131-17) duce desired shades of color in smoking products is well known. Several patents dislcose the use of vegetable dyes to control the color of tobacco. Such dyes have also been used in preparing tobacco sheets from finely ground tobacco and adhesives of various sorts.

Most useful dyes are water-soluble. Thus when in contact with saliva from the smokers mouth dye tends to dissolve out of the tobacco product at a rate significantly greater than the natural pigments of tobacco. This results in an undesirable dark shade at the head end of the smoking article.

The use of water-insoluble pigments and dyes overcomes some of the solubility problems. It has, however, been found that these products often have other objectionable qualities. For example, 2-(2-quinolyl)-1-3- indandione (Drug and Cosmetic Yellow #11) although producing good, colored tobacco products, has a tendency to sublime and produce a yellow colored smoke. Use of iron oxide pigments, for example, results in reddish-yellow residues in the ash.

It has been known for some time in the dye industry that certain water-soluble dyes may be laked onto inert carriers such as alumina and thereby be converted to water insoluble forms.

In the manufacture of tobacco it has been a common practice to incorporate ash and burn additives. A wide variety of such compounds as diatomaceous earth, bentonite, asbestos, montmorillonite clays, kaolin, and silicious particle materials of various types, have been used for this purpose.

It is an object of this invention to manufacture a smoking product characterized by the use of tobacco in combination with initially water soluble dyes which have been laked onto inert carriers useful for ash and burn control.

Another object of this invention is to provide a tobacco product, such as a sheet, in which tobacco is combined with an adhesive and reinforcing fibers upon which an initially water soluble dye has been laked to make the dye insoluble.

'and washed free of sulfate ions.

2,977,254 Patented Mar. 28, 1961 A further object of this invention is to form insoluble dyestuffs from water soluble dyes, readily combined with tobacco in aqueous systems commonly used in the manufacture of tobacco.

Contrary to the well known technique of laking on alumina, a superior product may be obtained according to this invention by forming the lake on a carrier which can later have double utility, namely to cause the dye to be uniformly distributed in an insoluble form and also to give control over the texture and color of the ash when tobacco containing the lake or lakes, is used either as wrapper or binder for cigars or as filler for cigarettes.

In the following examples, IA-D and IIA-C illustrate how to prepare pigment for'use in tobacco manufacture.

Example I-A Twenty gms. of aluminum sulfate were dissolver in 200 cc. of hot water and 32 gms. of an amorphous diatomaceous earth was added. The mass was agitated for 15 minutes and cooled to room temperature. To the above, gms. of aqueous 10% sodium carbonate solution was added slowly, stirred for 30 minutes, filtered,

The filter cake was resuspended in 200 cc. of water and 1.4 g. of the trisodiurn salt of 3-carboxy-5-hydroxy-l-p-sulfophenyl-4-p-sulfophenylazopyrazole (Food, Drug and Cosmetic [RD and C.], Yellow #5), dissolved in 100 cc. water, was added slowly to the suspended cake material. After 30 minutes a 10% solution of aluminum chloride was added in small quantities up to a total of 5-9 cc. while titrating tests were made after each addition to determine when the dye was fixed. The color is usually fixed when the pH of the charge is lowered to 5.5 by sufiicient amounts of aluminum chloride.

After complete fixation of the color the batch was stirred gently for 30 minutes and then filtered. The filter cake was washed twice with 100 cc. water in a filtered device to form a dye preparation. The pigment can be used in its wet form with tobacco.

Example I-B The base was prepared as in Example I-A. The FD. and C. Yellow #5 was replaced by the disodium salt of 1-pseudocumylazo-2-naphthol-3-6-disulfonic acid (RD. and C. Red #1). A pigment resulted which was of bright red color with very good fixation characteristics and fastness.

Example I-C The base Was prepared as in Example I-A. The PD. and C. Yellow #5 was replaced by the trisodium salt of 1-(4-sulfo-l-naphthylazo)-2-naphthol-3,6 disulfonic acid (RD. and C. Red #2). A pigment resulted which was of bluish-red color and had good bleed resistance and fair fixation characteristics.

Example l -D mixing continued for 30 minutes. A homogeneous uniformly colored filter cake was obtained. This was washed twice with 100 cc. water. The product was comparable in tinctorial power to material made according to Example I-A.

In addition to diatomaceous earth, the dyes shown above can be laked out on bentonite, silica gel, kaolin, and other inorganic carriers. The resulting products are similar to the diatomaceous earth lakes but result in some difierences in properties of tobacco products. For example, the bentonite lakes produce an extremely coherent, non flaking ash which is a desirable characteristic for cigars.

Additional water insolubility and bleed resistance of these lakes can be achieved through the use of rosin sizings in the lake preparation.

In addition to the process described above, the lake may also be prepared in such a way that the color is adsorbed on cellulose fibers which can be used for reinforcing tobacco films. The following are examples of this technique.

Example IIA A pulp consisting of pounds of refined cellulose fibers, which may be from tobacco, in 200 pounds of water was treated with one pound of a 1% by weight solution of ED. and C. Yellow #5. To the suspension The procedures shown in Example IIA were followed with the exception that the dye was the disodium salt of 4-[ [4- (N-ethyl-p-sulfobenzyl amino) phenyl] (4-sulfoniumphenyD-rnethylcne] [1-(N-ethyl-N-p-sulfobenzyl)- 13 cyclohexadienimine], (ED. and C. Green #2). The product was color fast and non-bleeding. A test sheet made from the fibers had excellent tensile properties and good color stability when wet.

Example I1-C The process of Example II-A was carried out, except that the dye was the disodium salt of 5,5-indigotin disulfonic acid (ED. and C. Blue #2).

The above lakes were used in manufacturing tobacco by processes illustrated below in Examples IIIV. Such tobacco may be used for wrapper on cigars, cigarillos, or little cigars, as binder for cigars, or as filler for cigars, cigarettes, or pipe tobacco.

Example 111 The process for laking ED. and C. Yellow #5 on diatomaceous earth shown in Example I-A was used to prepare 100 pounds of a wet filter cake containing 35% solids. The dye content of the lake was 3.5% on a dry basis.

A tobacco product was prepared according to the process described in Example I of US. Patent 2,887,414. The proportion of ingredients was identical except that 12 pounds of the 35% diatomaceous earth lake of Yellow #5 was added to the dispersion.

The resulting tobacco product was light tan in color as opposed to the deep brown of the control sheet. No noticeable differences in strength properties were found, but it was observed that the ashproduced when this product was used as a binder on cigars, was extremely coherent and light grey. Smoking quality was judged by a panel of experts to be superior to the untreated control cigar.

4! Example I V-A The green dyed fibers of Example II-B were used'to prepare a tobacco product in the following manner. The consistency of the fibers was adjusted to 2% by weight. A dry blend composed of one pound of carboxymethyl cellulose of a type having a 2% Brookfield viscosity of between 200 and 500 centipoises, two pounds of ground montmorillonite silicious catalyst, and 0.8 pound of polyglyoxal was dispersed into 200 pounds of the 2% fiber dispersion. After complete mixing, five pounds of tetraethylene glycol were added. To the resulting dispersion, 75 pounds of a 4% by weight solution of ethyl-hydroxyethyl cellulose of a type which as a 2% Brookfield viscosity of 1100 centipoises were added and mixed. The resulting adhesive solution was adjusted to 5% solids, was then continually mixed with a total of 25 pounds of tobacco powder which passed an 80 mesh screen to form a slurry while metering said slurry onto a continuous stainless steel belt with a casting knife. The thin uniform film was dried, remoistened, doctored from the belt, rolled up, and slit into bobbins for use on a wrapper feed device of cigar machines. The wrapper was somewhat greenish and had the appearance of a good Havana wrapper. Cigars made with this wrapper showed no discoloration at the heads, held up well on chewing, and smoked well with a resultant light grey coherent ash.

Example IV-B The process of Example IV-A was used except that the binding agent was locust bean gum and the fibers were derived from tobacco stems. Essentially the same results were obtained.

Example V Samples of wrapper-type tobacco which had been spotted by the well-known disease, weather-fleck, were treated by this invention. A yellow pigment was prepared according to Example I-A.

One pound of the pigment was dispersed in a solution composed of 2 lbs. of ethyl cellulose in 98 lbs. of a solvent containing 3 parts by Weight of benzene and one part by weight of methyl alcohol. After complete dispersion the pigment solution was sprayed on the wrapper leaves. After drying the resulting leaves had a light golden cast and were improved in quality. Cigars wrapped with the treated leaves were uniform in color and showed little or no evidence of the disease spots.

What is claimed is:

1. A smoking product comprising in combination an inert carrier, a water soluble dye mordanted upon said inert carrier and tobacco.

2. A smoking product according to claim 1 in which the carrier is inorganic.

3. A smoking product according to claim 2 in which Y the carrier is selected from the group consisting of diatomaceous earth, silica gel, bentonite, asbestos, montmorillonite clay, kaolin, and silicious particles.

4. A smoking product according to claim 1 in which the laked dye is selected from the group consisting of:

Trisodium salt of 3-carboxy-5-hydroxy-1-p-sulophenyl- 4-p-sulfophenylazopyrazole; disodium salt of l-pseudocumylazo-2-naphthol-3-6-disulfonic acid; trisodium salt of 1-(4-sulfo-1-naphthylazo)-2-naphthol-3,6 disulfonic acid; disodium salt of 4-[[4-(N-ethyl-p-sulfobenzyl amino) phenyl] (4-sulfoniumphenyl) methylene]- [1-(N-ethyl-N-p-sulfobenzyl) A cyclohexadienimine]; and disodium salt of 5,5-indigotin disulfonic acid.

5. A smoking product according to claim 1 which includes rosin size.

6. A smoking product according to claim 1 in which the carrier is cellulosic fiber.

7. A smoking product comprising in combination tobacco, a dye and an inert inorganic material upon which has been mordanted said dye material consisting of Yellow #5.

8. A smoking product comprising tobacco, a water tobacco, a dye and cellulose fibers upon which has been soluble dye and a cellulose adhesive upon which has mordanted said dye material consisting of Green #2. been mordanted said water soluble dye.

9. A smoking product comprising in combination References Cited in the file of this patent tobacco, a water soluble dye and dyed tobacco fibers- 5 upon which has been mordanted said water soluble dye. UNITED STATES PATENTS 10. A smoking product comprising in combination 1,756,778 Alden Apr. 29, 1930 tobacco, a dye and cellulose fibers upon which has been 1,863,813 Alden et a1 June 21, 1932 mordanted said dye material consisting of Yellow #5. 1,972,718 Sharlit Sept. 4, 1934 11. A smoking product comprising in combination 10

Claims (1)

1. A SMOKING PRODUCT COMPRISING IN COMBINATION AN INERT CARRIER, A WATER SOLUBLE DYE MORDANTED UPON SAID INERT CARRIER AND TOBACCO.