US3421519A - Reconstituted tobacco sheet - Google Patents

Description

United States Patent 3,421,519 RECONSTITUTED TOBACCO SHEET Raymond J. Moshy, Westport, Conn., and Felix J. Germino, Palos Park, 11]., assignors to American Machine 8: Foundry Company, a corporation of New Jersey No Drawing. Filed July 25, 1966, Ser. No. 567,358 US. Cl. 13117 3 Claims Int. Cl. A24f 47/00; A24b /00 ABSTRACT OF THE DISCLOSURE A reconstituted tobacco sheet having high tensile strength and water insolubility which is made by slurrying and then sheeting finely divided tobacco particles and deacylated chitin. The chitin may be mixed with plant gums and wet strength may be increased in the final product by cross-linking with an aldehyde.

The present invention relates to reconstituted tobacco composition. It particularly concerns the use of the substance chitin as an adhesive for tobacco particles.

A number of reconstituted tobacco compositions have found great commercial success as filler material for cigarettes or cigars and as binders or wrappers for cigars. These compositions have generally utilized natural plant gums or their derivatives, such as galactomannans and cellulose derivatives, as adhesives and/ or as coating films. The art relating to the use of these plant or vegetable adhesives is quite advanced and well known to those skilled in the art. It is believed unnecessary at the present time to include a discussion here of this art but reference is made to US. Patents 2,734,509, 2,734,510, 2,334,513, 3,185,161 and 3,185,162 for example.

It has been found that the plant gums or polysaccharides such as the cellulose derivatives or galactomannans are not entirely satisfactory in creating reconstituted compositions which are completely water insoluble or which have superior tensile strength or have high ammonia stability. Numerous attempts have been made and much money and etfort has been expended in order to overcome or ameliorate these problems by varying processing procedures or by employing numerous additives.

We have found a new material, deacetylated chitin, which either alone or mixed with other natural or derived plant gums, as an adhesive or as a film-forming coating, produces tobacco compositions of superior qualities. Deacetylated chitin, the degree of deacetylation being in the range from strong acid solubility to complete deacetylation, when dissolved in dilute acetic acid and subsequently mixed with tobacco and other optional ingredients form strong tobacco compositions having good dry tensile properties including wet and ammonia strengths. When chitin is used as a film forming agent it produces a sheet having high hydrophobic and water repellency properties.

In all instances We have found that using chitin has also resulted in tobacco compositions having very good smoking characteristics such as burn, aroma, taste, ash, etc.

Another advantage found in chitin is the fact that this material is rather inexpensive being derived from crustacean waste materials such as from the shells of shrimp, lobsters and crabs.

While we have found that chitin performs quite well by itself or with minimal amounts of other gums, we have also found that chitin reacts, mixes and is synergetic with these gums as well as with cross-linking agents. In fact cross-linking, if desired, seems to increase wet strength, dry tensile values and ammonia stability somewhat more than would normally be expected. Furthermore, we have found that the normal cross-linking materials and procedures are applicable to chitin.

Additionally, we have found that a periodate oxidized dialdehydecan be prepared from chitin, since the periodate reaction is applicable to compounds having two hydroxyl groups or hydroxyl and an amino group attached to adjacent carbon atoms. U.S. Patent No. 2,988,455 Rosenberg et al. discloses compositions of matter consisting of water-soluble polysaccharide film -forming ma terials in combination with a dialdehyde polysaccharide selected from a group consisting of starches, cellulose, galactornannans and dextrans. This patent does not include compositions of matter with dialdehydes obtained from amino-type polysaccharides (e.g. chitin, glucosamine, etc.) nor those obtained by reacting amino-type polysaccharides (e.g. chitin, glucosamine) with dialdehyde starches.

Accordingly, among the objects of the present invention are those which desire to overcome certain of the prior art problem, produce a new tobacco composition of exceptional quality and to do the same more economically than had been previously done.

These and other objects as Well as further advantages will be apparent from the examples that follow which describe and illustrate the present invention.

Chitin is a linear polymer of anhydro-N-acetyl-D-glucosamine (N-acetyl-Z-amino-2-deoxy-D-glucose).

In the folowing disclosure the form of chitin used is Kylan LV supplied by Morotex Chemical Company, Spartenburg, S.C.

Examples 1-7 illustrate the use of chitin as an adhesive.

EXAMPLE 1 Four hundred grams of a 4% Kylan in 2% acetic acid solution was transferred to a Waring Blendor and blended with sixteen grams of TEG (tetraethylene glycol). Sixtyfour grams of tobacco and fifty grams of water were added and the whole blended again. The final slurry contained 20% solids and had a viscosity of 11,600 cps. at 96 F. This slurry was cast on a continuous, moving stainless steel belt, at a 10 mil knife clearance, at a belt speed of 11.5 ft./ min. The sheet was partially dried in gas-fired impingement ovens and completely dried on a steam box. The sheet was rehumidified and doctored from the belt.

Physical Properties Sheet wt g./ft. 4.7 Percent moisture percent 26.5 Longitudinal dry g./in 1 360 Transverse dry g./in 340 Longitudinal wet g./in 2 Longitudinal NH g./in Porosity sec 30 1 S9% stretch. 2 13-14% stretch.

EXAMPLE #2 Formulation One hundred and twenty grams of a 4% Ethulose (ethylhydroxy-ethylcellulose) solution and 280 grams of 4% Kylan in 2% acetic acid were transferred to a Waring Blendor. TEG (tetraethylene glycol), tobacco, and water were added as in Example #1. The final slurry contained 20% solids and had a viscosity of 1=l,600 cps. at 69 F. Casting and drying conditions were as in Example #1. The sheet was remoistened and removed from the belt.

3 Properties Sheet wt g./ft. 4.57 Percent moisture percent 23.1 Longitudinal dry g./in 1 285 Transverse dry g./in 260 Longitudinal wet g./in 2 95 Transverse wet g./in 95 Longitudinal NH g./in 105 Porosity sec 135 1 12% stretch.

15% stretch.

EXAMPLE #3 Three hundred and fourteen grams of 2.5% paper pulp in water was transferred to a Waring Blendor. Eight and four tenths grams Kylan (corrected for 5% moisture) and 4 grams of glacial acetic acid were added and blended in, followed by 48 grams of tobacco, 8 grams TEG (tetraethylene glycol) and 171.6 grams of water. This final slurry containing 13% solids was blended until smooth. Casting and drying were the same as for Example #1 except for the belt speed and knife clearance. The knife setting was at 15 mils and the casting belt speed 45 ft./min. The drying belt speed was 7 ft./min. The sheet was remoistened and doctored from the belt.

Properties Sheet wt g./ft. 5.44 Percent moisture percent 20.5 Longitudinal dry g./in 1 880 Transverse dry g./in 360 Longitudinal wet g./in 2 480 Transverse wet g./in 180 Longitudinal NH g./in 470 Porosity sec 6 1 6% stretch. 2 6% stretch.

EXAMPLE #4 Three hundred and fourteen grams of 2.5% pulp in water was transferred to a Waring Blendor. Six and seven tenths grams of Kylan (corrected for 5% moisture) and 3.2 grams of glacial acetic acid were added and agitated until all the Kylan was dissolved. Forty grams of 4% Ethulose (ethylhydroxyethylcellulose) solution and eight grams of TEG (tetraethylene glycol) were then added and blended in, followed by 48 grams of tobacco and 134.1 grams of water. This final slurry containing 13% solids was blended until smooth. Casting and drying were the same as for Example #3. The sheet was rehumidified and removed from the belt.

Properties Sheet wt g./ft. 4.64 Percent moisture percent 17.8 Longitudinal dry g./in 1 830 Transverse dry g./in 2 95 Longitudinal wet g./in 2 330 Transverse wet g./in 150 Longitudinal NH g./in 370 Porosity sec 130 1 5% stretch.

2 5% stretch.

EXAMPLE #5 One thousand eight hundred and eighty-two grams of 2.5 pulp in water was transferred to a steel container. Eighty and six-tenths grams Kylan (corrected for 5% moisture) and 3 8 grams of glacial acetic acid was then added and this mix blended in an Eppenbach mixer until all the Kylan was dissolved. Seventy-two grams of TEG (tetraethylene glycol), 32.6 grams of Dicalite (brand of diatomaceous earth manufactured by the Great Lakes Carbon Co.), and 2000 ml. of water was then added and blended in. Six hundred and six grams of tobacco (corrected for 5% moisture) and pre-wetted with 1158 ml. of

water was then added and blended in followed by 480 grams of 4% Ethulose (ethylhydroxyethylcellulose). The final slurry was then homogenized. The final slurry contained 13% solids and have a viscosity of 6,700 cps. of 40 C.

Casting and drying conditions were the same as in Example #1 with the casting knife clearance at 17 mils and the belt speed '8 ft./ min. The sheet was rehumidified and removed from the belt.'

Properties Sheet wt. g./ft. 5.0 Percent moisture percent 20.6 Longitudinal dry g./in 1 715 Transverse dry do 410' Longitudinal wet do 250 Transverse wet do Longitudinal NH do 280 Porosity sec 43 1 7S% stretch. 2 9 stretch.

EXAMPLE #6 Eight grams of Kylan was added to 250 grams of water and 10 grams of glacial acetic acid in a Waring Blendor. The mixture was blended until all of the Kylan was dissolved. Two and four tenths grams of Dicalite and 8 grams of polyglycerine were added and blended. Thirtytwo grams of tobacco was then added and blended. The final slurry contained 16.2% solids.

Hand sheets were cast from this slurry on glass plates with a 14 mil knife and dried at 300 F. in an electrically heated oven. The sheets were rehurnidified and removed from the glass plates.

Properties Sheet weight g./ft. 5.5 Longitudinal dry g./in 1 400 Longitudinal wet g./in 2 280 Longitudinal NH g./in 295 1 5% stretch. 2 30% stretch.

The following example using glyoxal cross-linking of a deacetylated chitin tobacco sheet is illustrative of the effect of cross-linking of chitin films with an aldehydic reagent, and is compared to the untreated material. Notice here that the amount of glyoxal used is very small. Increasing the glyoxal level will increase the tensile values.

The following illustrates the use of chitin, cross-linked with a glyoxal, as an adhesive.

EXAMPLE #7 Six grams of deacetylated chitin was dissolved in 27.0 ml. of water containing 20 ml. of glacial acetic acid. To this gum solution, 4.2 grams of Dicalite, 4.5 grams of TEG (tetraethylene glycol) and 250 grams of 2.5% paper pulp in Water was added and blended in a Waring Blendor. After blending for a few minutes 96 grams of tobacco was added and blended for several minutes. The sample was cast on a glass plate with an 8 mil casting knife and dried at 300 F. The sheet was removed after remoistening.

Sheet weight 4.5 grams.

Results after overnight equilibration were:

G./in. Transverse dry 312 Transverse NH 165 Transverse wet 208 Three grams of deacetylated chitin was dissolved in 135 ml. of water containing 10 ml. glacial acetic acid to the gum solution. 2.1 grams of Dicalite, 2.8 grams of TEG and grams of 2.5% paper pulp in water was added and blended in a Waring Blendor. After blending for a few minutes 48 grams of tobacco was added and blended for several minutes. 1 ml. of 30% glyoxal was added and the sample immediately cast with an 8 mil knife on a glass plate.

The sample was dried at 300 F., the sheet Was removed after remoistening and equilibrated ovemight. Sheet Weight 4.5 grams.

G./in. Transverse dry 460 Transverse NH 210 Transverse Wet 260 2. The reconstituted tobacco sheet of claim 1 including a cross-linking agent.

3. The reconstituted tobacco sheet of claim 1 in which the chitin is in the form of an oxidized dialdehyde.

References Cited UNITED STATES PATENTS 2,099,363 11/ 1937 Heckert 117144 3,042,552 7/1962 Rosenberg et a1. 131-140 X 2,047,226 7/ 1936 Rigby 154-2 MELVIN D. REIN, Primary Examiner.

US. Cl. X.R.