DE1767523A1 - Process for making reconstituted tobacco products - Google Patents

Description

MÖHLSTRASSE 22, CALL NUMBER 48 3921/22

American Machine and Foundry Company, New York, USA

Process for making reconstituted tobacco products _ ^

The invention relates to a method of making reconstituted Tobacco leaves and, more particularly, to an improved process for making light colored reconstituted tobacco leaves; despite the use of heat as a manufacturing aid at certain stages of the process.

The technical process for making reconstituted tobacco leaves requires the application of heat at certain stages of the process, such as either the manufacturing steps and / ■ or when drying. It is known that the color of the finished tobacco product darkens due to the heat treatment, the (Jrad des Dunkeins is a function of temperature and heating time. As a rule, it is desirable to make a brightly colored tobacco leaf, and it different steps have been taken to achieve this goal, such as the addition of dye chemicals, the addition of Furbe-Mankierun ^ sini tteln ("7 / eißmaehern"), such as titanium dioxide or "13icalite", or temperature control and heating time control.

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However, these tuck rides are never entirely satisfactory because of the limitations under which they can be used. By doing In the case of the addition of coloring and masking chemicals, the addition of foreign matter may be undesirable, especially if excessive Quantities are required to achieve the desired results. Excessive use of τοη dyes can cause "eye-sight" problems ("leaohing problems ") Terursaohen, while excessive use τοη" whiteners " can lead to leaves that are gray in appearance or lack the correct physical structure. In the case of controlled temperature and heating time, there are undesirable limitations in relation to the manufacturing process. The one revealed here Invention makes the manufacture of a brightly colored reconstituted Tobacco leaf with no added coloring for color retention and without any undue limitation on temperature and exposure possible in the process. This is achieved by selectively removing from the tobacco the special agents that darken the tobacco are responsible for warming.

In the production of additional "constituted tobacco, tobacco, such as, for example, stalks and stalks, scrapings, whole tobacco leaves and the like, preferably evenly comminuted or ground and shaped into tobacco leaves which are suitable for later masohinelle processes. On the other hand, in the production τοη each tobacco reconstituted leaf or in the case of reconstituted tobacco leaves where efficient utilization of the natural tobacco gums is desired let, the tobacco usually by a wet process or by friction or

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Refining ground into particles of colloid-forming size. However, the great amount of energy and time required to produce these tobacco particles of colloid-forming size has the application of these processes to the manufacture of reconstituted tobacco leaves limited.

In order to reduce the amount of tobacco used to crush the tobacco particles in the wet process To reduce energy and time taken, it is desirable to expose the tobacco to heat before refining. These Heat treatment reduces finishing time and at the same time improves the physical properties of the finished product. The heat treatment however, darkens the tobacco and therefore darkens the tobacco leaves made from this heated tobacco material, thereby rendering such leaves useful in a number of tobacco manufacturing products be made unusable.

Much effort has been made to date to reconstitute tobacco leaf with the application of heat at certain stages of the process without the unfavorable darkening of the tobacco occurring. It Various techniques and processes have been used, but in general these efforts have had limited commercial success had. For example, it is known that a relatively good product in terms of color is obtained if the tobacco products are pre-treated are washed with water, the wash water is replaced with fresh water and then the washed tobacco is heated. This method however, it is unsatisfactory from an economic point of view, since the discarded wash water contains a large amount of useful tobacco pro-

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contains.

The invention proposes a solution to this long-standing problem and, as a result, brings about a considerable saving in energy and time that are good for obtaining reconstituted leaf tobacco Quality and excellent color are required.

Another object of the invention is a method for manufacturing a light colored W lung reconstituted tobacco sheet in spite of the application of heat as a manufacturing aid to be indicated.

To remove tobacco before there is another object of the invention is also to remove polyphenols from the / Tobacco-water mixture in the manufacture of the reconstituted tobacco leaf without resorting to dye and dye chemical additives to tobacco exposed to heat.

Another object of the invention is to remove only the agents from the tobacco before the tobacco-water mixture is exposed to heat P which cause the tobacco to darken, and to leave all other valuable material in the tobacco without adding anything to the tobacco to achieve a brightly colored tobacco leaf.

Another object of the invention is to propose a method of performing the above, which can be used in the manufacture of large Quantities of tobacco can be applied and a reconstituted tobacco leaf provides excellent color, in an economical and easily controllable way.

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Other objects and advantages of the invention will appear from the following.

For the purposes of the invention, tobacco includes any type of tobacco that is used for production of reconstituted tobacco leaves, such as stems and stems, leaf veins, beetles and tobacco waste, rejects etc., and also whole leaves and parts of them.

In general, the invention proposes a method for removing the mit ™ tel from the tobacco washing water before that for the darkening of the tobacco, if exposed to heat are responsible. The treated Wasohwasser are then returned to the tobacco to be manufactured and the product is manufactured in a manner known per se to obtain a reconstituted Tobacco leaf with good physical properties with no Naohteil on the Leaf color to deliver.

It has long been widely believed that the one responsible for the obscurity of the The substances responsible for heating tobacco are the carbohydrates and the Are amino acids that react to form dark colored compounds upon heating; the process is called the "Laillard reaction". However, it has been found that neither the carbohydrates nor the Amino acids significantly darken tobacco when heated, but that in tobacco contained polyphenols, especially the basic polyphenols, a considerable amount Darken the tobacco after exposure to heat. This· Appearance is also pH-dependent.

A number of attempts have been made to isolate and determine the agent

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which cause the tobacco to darken after heating. The following procedure shows how the polyphenols were identified as the agents that cause the tobacco to darken during heating.

A sample of 10 g of Brighf stem dust was distilled with 90 ml Water mixed. The slurry was filtered on a Buchner funnel using Whatman # 1 filter paper. The filter cake was then mixed with 90 ml of a predetermined liquid and the Mash brewed into a vessel, such as an earthenware vessel, which was sealed and placed in a pressure cooker, where there were two Heated at about 120 ° C at about 1.05 kg / cm2 for hours. After cooling, there were 3 tobacco leaves with a thickness of about 0.23-0.30 mm poured from the pulp onto 20 cm χ 20 cm glass plates. The leaves were dried in an oven at 110 to 115 ° C for about 15 to 20 minutes, and the color of each sheet was examined in a Gardner automatic colorimeter (model AC-2A, 200 series). Readings were taken by placing the plate over the gardner opening so that the tobacco side faces the opening. A number of readings were taken taken at different points on each plate in order to obtain an overall consistency.

The test results in Table 1 were with various additives in the predetermined liquid and serve to clarify that polyphenols are the agents that darken the tobacco when exposed to it Cause heat. In all cases water washed bright stem leaves were used, unless otherwise stated. The weight

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of the washed tobacco in each sample was 7 »0 g dry weight and this was suspended in 90 ml of liquid before heating.

Table 1

Color of tobacco leaves made from "bright" stalk pigeon, heated in solvents containing various additives

materials

pH value pH value Rd before after
Heating heating

a +

b +

Washed tobacco + water 5 »3 (positive comparison)

Unwashed tobacco + water

Washed tobacco + washing water (negative comparison)

Washed tobacco + sucrose (2g) + water

Washed tobacco + glucose (2g) + water

Washed tobacco + fructose (2g) + water

Washed tobacco + succha 7.2 rose, fructose, glucose (2g each) + water

Washed tobacco + tryptone 6.3 (1g) (casein extract) + water

Washed tobacco + tryptone 6.1 + sucrose (1g each) + water

Waxed tobacco + tryptone 6.1 + SeeGlukese (1g each) + water

24.9 3.1 21.5

3.8 16.3 4.0 16.4

25.4

25.2

24.7 26.8

22.5 2.7 16.3

22.9 2.5 17.3

22.2 3.3 17.5

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Table 1 (continued)

Color of tobacco leaves made from "bright" stem dust, heated in solvents that contain various additives

Materials pH value pH value Rd a + b +

before heating after heating

Washed tobacco + tryp- 6.1 - 22.0 2.5 17 »1

clay + fructose (1g each) +

water

Washed tobacco + tryp- 6.2 - 21.9 3 »8 18.2 ton + glucose, fructose, Sucrose (1g each) + water

Washed tobacco + water 5.2 4.5 22.6 3.5 16.3 ser + acid polyphenols

Washed tobacco + water 9.3 6.3 12.4 5> 8 15 »0 aer + basic polyphenols

Washed Tobacco + Was- 5.7 4.8 17.2 4.7 16.1 ser + acidified basic polyphenols

Washed tobacco + Pb- - - 23.4 -acetate solution (10%) water

Comment » Rd« Holiness factorj black ■ Oj white - 100

^{a +} " γ coordinate components on a color value diagram

b + - J

Pb acetate = lead acetate

The polyphenol fractions shown in Table 1 were obtained as follows »

90 ml of a tobacco-water extract, prepared as described above, were mixed with 20 ml of a 10% lead acetate solution and the resulting solution Precipitate was removed by centrifugation. This precipitate

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contained the acidic polyphenol fraction.

Add more lead acetate solution to that separated from the lower base Solution no longer caused precipitation. An alkaline Reactants, such as ammonium hydroxide (NH.0H), from this Liquid added until the pH was about 8.5 to 9.0. The precipitate formed, collected by centrifugation, made the base level Polyphenol fraction.

As can be seen from the experimental results shown in Table 1 the basic polyphenols give a darker leaf than even the negative comparison sample (brightness factor readings 12.4 or 16.4) It can also be seen that although acidification of the basic polyphenols improves the color, they are still far below the positive comparison (brightness factor readings 17 »2 and 24.9, respectively) · These results show furthermore that the sugar and amino acids do not affect the color of the tobacco leaves influence and in a similar way also do not affect the precipitation of the polyphenols lead acetate solution used.

Process for neutralizing or removing the polyphenols from tobacco by adding chemical substances are in the application filed on the same day as the present application in USA with the serial number 639 066. The present description is therefore limited to the removal of polyphenols without chemical substances.

To get the basic polyphenols from the tobacco without adding any ohemlsohen To release (leach out) additive to the reconstituted tobacco leaf,

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The tobacco wash waters can be treated with adsorbent material that does not add anything to the extract, but which selectively removes the agents that cause the tobacco to darken through adsorption. For example, tobacco wasoh water is passed through a column that is a contains selected adsorbent material, such as activated alumina. The adsorbent removes the darkening material, but leaves it other valuable tobacco bed parts unchanged in the extract. The treated extract is then made with the original, washed tobacco and the combination is processed into a reconstituted tobacco leaf which has its light color, useful in the tobacco industry, without additives.

According to the invention, untreated tobacco such as broken leaves, saplings, stalks and stems or trunks become various Fractions or waste and scrap, subjected to a water extraction process to separate off the water-soluble components.

The water-soluble components of the tobacco or the extract are made by any suitable method, such as draining, pressing or centrifugation, is separated from the insoluble part. Of the Aqueous extract contains various water-soluble substances, including polyphenols. This aqueous extract can then be poured through a column containing an adsorbent material such as activated alumina. It can operate in one continuous mode Column can be effected by introducing the adsorbent material and continuously passing the aqueous extract through a column. That

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adsorbent material removes the color-forming body, but leaves it

the other valuable tobacco components unchanged in the column bed ..

run. The column drain is then with the originally washed tobacco combined and the combination is further treated by methods known per se; it becomes a light colored reconstituted tobacco leaf manufactured. The extracted or leached coloring materials can be eluted from the adsorbent so that, if desired, they can be reused or reconditioned. -

In the following, preferred exemplary embodiments are explained in more detail described.

A glass column (25 cm 3 cm) was activated with a slurry of 100 g Aluminum oxide (1.40 to 2.35 now) filled in water. The water was draining off and the column was repeatedly washed with about 500 to 1000 ml of fresh water. A water extract from tobacco pigeon, as before has been prepared as described, was sent through the column at a flow rate that 0.5 »1 column drainage per minute were collected. The column was then washed with water until the wash water was colorless. The combined wash water and the collected Column effluents were then concentrated to 100 ml under vacuum in a flash evaporator using a temperature range of 36 to 38 ° C. The solids content in the concentrate as well as in the original Waeeer tobacco extract was determined and the recovery of material from the column was calculated from these values. The test results are in Table 2 compiled.

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Table 2

Solids in tobacco water extracts and in the column drain ¹ of aluminum oxide columns

Sample tobacco solids solids solids

stem in the H ₉ O-Ex-
tract \ jfil on the pillar
given CfI in conc
treaded
Column blueprint
fen back
won f «! J Again
acquisition 1 Bright 4.50 9.00 6.73 74.5 2 Il 4.57 9.14 6.72 74.5 3 Il 4.52 9.04 6.52 72.5 4th Il 4.55 9.10 - - IfN Penn. 3.17 6.34 - - 6th Il 3.15 6.30 5.63 89.2 7th Il 3.15 6.30 5.64 89.3 8th It 3.14 6.26 5.67 90.5

Table 2 shows that the solids recovery 73 to 75 fi for Bright-stem-Extraktβ and 89 to 91% for Penn.-stem extracts is.

The material not removed from the column by washing water was eluted, by pouring 2-normal formic acid through the column. Factions were collected at a rate of 0.5 ml per minute. the eluted samples were very dark in color. The 2 normal formic acid removed all adsorbed material and left the activated alumina

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free of color back. The aluminum oxide was washed with water until it was acid free, ^{dried in an oven (130 to HO 0} C) overnight and then used again.

The formic acid was removed from the eluate (i.e. the basic polyphenols) removed by evaporation in vacuo on a flash evaporator. The remaining dark brown material was washed up with water a volume of 100 ml was added and carbohydrates through a Thin layer chromatography methods investigated, as reported in the "Journal of Chromatography "_1J3, 170 to 174 (1965). Samples of the Column effluent concentrates referred to above, as well as the original tobacco water extract were also tested for carbohydrates. The results showed that practically all carbohydrates those found in the original tobacco water extract were recovered in the concentrated column effluent, while only insignificant ones Amounts were found in the formic acid eluate.

It should be noted that the material, which is not affected by water from the column could be removed by other suitable solvents, such as 50 ^ iges ethanol containing 2-normal HCl, or by 2 normal HCl solution, could be eluted. Formic acid is advantageous preferred because it is easily removed by evaporation under vacuum. This makes the recovery of the solids from the formic acid eluate possible as well as their subsequent use in the dye experiments. In a process in which these solids are inconsequential, their removal from the aluminum oxide would be more economical with 2 normal HCl solution are executed.

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-H-

The column effluent concentrates were taken up to a certain volume and combined with the washed tobacco. The pulpy mixtures were treated as described above. The tobacco leaves obtained were examined in a Gardner colorimeter} the results are in Table compiled.

Tabel

Gardner readings on tobacco leaves marked with various Column drains and eluates made from aluminumocide columns became

tobacco (Positive-
Comparison) Penn " (Positive ver
same) fraction PH value
of tobacco
Porridge Rd a + b + Bright (Negative-
Comparison) Il (Negative ver
same) Column drain con
centrate 5.8 21.5 •
3.7 17.5 ti Il Il 5.6 24.6 - - Il Il Il 4.7 24.6 5.4 34.4 Il Formic acid
Eluate 3.2 17.4 4.1 22.7 It - 5.3 24.8 3.9 35.0 It - 4.8 16.8 4.8 22.3 Column drain con
centrate 6.3 19.6 5.0 24.6 Formic acid eluate 3.8 17.1 6.1 23.3 - 7.0 19.3 5.2 24.6 - 6.2 17.4 5.3 22, fi

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- 15 -

Table 3 (continued)

Gardner readings on tobacco leaves marked with various Column drains and eluates from alumina columns were prepared

Tobacco fraction pH value Rd a + b +

of tobacco pulp ■

Bulgarian column drain - 5.1 15.8

concentrate

(Positive - 5.7 15.5

Comparison)

"(Negative- - 5.2 11.3

Comparison)

Comment »The positive comparison consists of natural tobacco (7g weight dry) plus fresh water

The negative comparison consists of washed tobacco plus the wasoh water obtained

Table 3 shows that the ^ effluent concentrates from the absorbent column in their Color properties are similar to the positive comparison, while the formic acid eluate, after removal of the formic acid and volume adjustment with Water that are similar to the negative comparison. This is particularly evident in the lightness values (Rd values).

Adsorbents other than activated alumina have also been investigated. Regenerated alumina worked as well as unused alumina. Polyamide and silica gel also gave satisfactory results.

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Other adsorbent materials could also be used, such as magnesol, kteelic acid or adsorption aluminum oxide and the same. However, these materials are finely grained and easily cake together in the columns so that the flow through the columns is reduced will. A pressure source would be required when using these adsorbent materials to provide adequate flow through the column to obtain. It should be noted that the preferred adsorbent materials need not be used in a column. You can also used effectively in pulp-type removal processes for polyphenols will.

According to the method according to the invention, a reconstituted tobacco leaf is made manufactured under the application of heat, which contains all the desirable parts of the original tobacco and which is lighter in color than leaves made from untreated tobacco.

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Claims (10)

Claims 1. Reconstituted tobacco, characterized in that the Polyphenol-Bestestand.il is at least partially removed. 2. Tobacco according to claim 1, characterized in that the basic polyphenol component is removed. 3. A method for producing tobacco in the production of reconstituted tobacco products, characterized in that that the water-soluble components including the polyphenols are leached from the tobacco, the aqueous extract solution containing the polyphenols from the leached tobacco is separated, at least part of the polyphenols from the Extract solution is removed, the extract solution from which the Polyphenols are at least partially removed with the leached Tobacco is combined, a pulp is formed from the water-tobacco mixture, and the pulp is brought into the desired shape and drying the molded tobacco pulp. 4. The method according to claim 3 »characterized in that the basic polyphenols are removed. 5. The method according to claim 3, characterized in that the polyphenols are removed by the separated extract solution is brought into contact with an adsorbent material which is used to selectively remove the polyphenols from the extract solution suitable is. 109843/1392 6. The method according to claim 5, characterized in that activated aluminum oxide, polyamide, oilicagel, magnesol, silica, or adsorption alumina is used. 7. The method according to claim 5 or 6, characterized in that the adsorbent material is arranged in a column and the extract solution is sent through the column. 8. The method of claim 5 to 7, characterized in that the adsorbent material is regenerated to the adsorbed polyphenols to remove, and that the distal adsorbed material is discarded. 9. The method of claim 5 to 7, characterized in that the spent adsorbent material is treated with a solvent for basic polyphenols, to elute the basic polyphenols from the adsorbent material, and that the treated adsorbent material is dried. 10. The method according to claim 3, characterized in that the re-formed water-tobacco mixture before the formation of the pulp is heated. 1Ü98A3 / 1392