DE2913354A1 - METHOD FOR PRODUCING A CELLULOSE FIBER - Google Patents

Description

.- ■ - rr \ ', tp

Dr. rer ϊϊιΙ Ί "jioinds Beroadl Γγ.-Τμ «H-AR3 Leyh

Lucile-Grohn-Siiaf: «38 D 8 Munich 80

P 322-125

Billerud Uddeholm AB Dr Be/sa

Billerud Uddeholm AB SÄFFLE, Sweden

Process for the production of a cellulose fiber

fabric

IÖ98U / 07S

description

The invention relates to a pulp, paper and their production. According to one embodiment of the invention relates to this a new cellulose fiber material, which is mainly made of wood, and a process for the production of paper that contains this pulp, *) The invention also relates to paper that contains the new pulp This paper contains a low air resistance, a high opacity and a good absorption capacity for fillers owns. The invention also relates to products made with the new paper, and especially cigarettes made with the new paper.

According to the prior art, wood pulp has only been used to a certain extent for the manufacture of cigarette paper used. The reason why such fibers have not found widespread use is that this pulp could not meet the requirements that are made of a pulp for cigarette paper QualüSt are made, these requirements being frequent are difficult to combine. Of these requirements it can be mentioned that the pulp as possible should not give the finished cigarette an unpleasant taste. The cigarette paper should have a large porosity have, i.e. a low air resistance, which is why is important so that the cigarette does not go out by itself.

*) However, according to a broader scope of the invention, other cellulose raw materials are taken into account, such as grass, straw and other parts of plants.

9098A2 / 0761 _ ₉ _

Low air resistance is also provided to reduce tar build-up. Furthermore, the fiber should have a high absorption capacity for fillers ". This promotes the opacity as well as the desired brightness of the cigarette ash, Other qualities considered essential are, for example, the tear-off length and the capillary Climbing ability, i.e. the ability to soak up water or solutions, which is a measure of the paper's ability to absorb certain chemical preparations. A high capillary climbing ability also acts to soften the paper due to the absorption of saliva.

So far, the requirements placed on a pulp for cigarette paper have been best met by the

eiy
Use of fiber based on flax and / or hemp is sufficient. Fibers made of flax and hemp are superior because they have a very high opacity and very low air resistance and at the same time have a very good absorption capacity for fillers and mechanical workability. However, flax and hemp also have significant disadvantages. For one thing, its price is very high. In addition, the quality fluctuates depending on the weather during the growing season and the changing cultivation and harvesting methods of the farmers and depending on the difficulties in adapting the digestion, drying and bleaching to the fluctuations in the raw material. In addition, deliveries are extremely unsafe for a number of reasons. Therefore, pulp from flax and / or hemp has been mixed to a significant extent with pulp from wood, primarily pulp for normal paper manufacture. So-called alpha fibers, ie a heavily bleached sulfate fiber with a high content of alpha cellulose and a low resin content, were also used, as is described in DE-PS 844 250. Such a fiber material can through

909842 / 075-

- 10 -

Treating sulphate pulp with strong cold NaOH solution (6 to 10 %) . The cold alkaline treatment, also known as mercerization, dissolves the hemi-cellulose and increases the alpha-cellulose content. As a result, the resistance to the passage of air is reduced and the opacity of the finished paper is improved, but without reaching the values which are required in the case of high quality requirements for cigarette paper. At the same time, the capacity for absorbing other substances is also drastically impaired, as is the mechanical workability and structure to a considerable extent. The use of alpha pulp for the manufacture of cigarette paper has therefore essentially ceased, or at least has been reduced significantly.

The object of the invention is to create a process for the production of a new cellulosic fibrous material based on wood, this process requiring considerable outlay on equipment, requiring no substances of any kind supplied from the outside, or requiring no significant expenditure of energy. These and other objects can be achieved in that a starting material which has been made essentially of wood is mechanically processed, essentially without prior cold alkali addition, in a strongly alkaline aqueous solution, by which is meant an aqueous solution, the OH-bearing cations in an amount which, in the case of NaOH, corresponds to an amount of 20-100 g, preferably 30 to 80 g, NaOH per liter of solution. In addition to NaOH, other alkaline compounds can also be used in aqueous solution, such as NH, (= NH ^ OH), KOH and Mg (OH) ₂ . A mechanical device in which the fiber material is processed is expediently used

009842/076 "?

essentially without cutting, this device belonging to the group consisting of frotapulpers, disc refining devices, Jordan refiners, Dutch and pan mills. A Frotapulper is most useful used for mechanical processing. Although "Frotapulper" is a commonly used name for a device is used in the paper and pulp industry is ", (cf. Paper Trade Journal, September 1, 1975) a more precise definition is given. A Frotapulper consists of a housing with an inlet opening and an outlet opening and two screws, which are arranged in the housing are and interlock. The material continuously fed in from one end of the device becomes kneaded (rubbed) between the edges of the snails. Another name for this type of device is "Frottator". An older type of device that has a slightly different construction but operates in a similar manner is also shown below known as the "Curlator". These devices have in common that they process the material without cutting, namely knead or scrub. They are similar in that regard the now obsolete pothole. In the strongly alkaline aqueous solutions, the fibers swell strongly, what with an alkaline treatment is normal, especially with the cold alkali conclusion, but go after the mechanical one Processing and then washing the fibers according to the invention back to their normal strength. By the mechanical processing in the strongly alkaline environment, however, the fibers are partially split, but in the essentially without being fully fibrillated or cut. In particular, the fibers should be strong though expediently not swollen up to the maximum before the cold alkali splitting be. One might fear that the mechanical treatment of the strongly swollen fibers in a disc

SÖ9842 / O7S1 " ¹² "

Refining device, frotator, or similar device leads to the fact that the fiber breaks down completely and is broken down into very small particles, the are no longer able to form paper of any strength. However, the invention has shown that this Risks can be avoided assuming that the mechanical processing of the heavily swollen fibers takes place certain specified conditions is carried out, these conditions e.g. the choice of the appropriate fiber concentration and temperature and the adaptation of the energy and power supply to the alkaline strength and fiber concentration as well as the type of device used in each case. During the mechanical processing according to In the invention, the fibers are partially split to form continuous fibril packets or bundles, which are important for the structure of the new fiber material according to the invention. With the new fiber they can Fibril bundles to a greater extent also form single fibrils be split up.

A fiber material obtained by chemical, semi-chemical and / or thermomechanical digestion is used as the starting material, which is obtained essentially from wood, preferably essentially a sulfate pulp used. Have attempts has shown that it is possible to produce the new pulp according to the invention starting from a starting material of this type by mechanical processing in a device, the fiber material being subjected to mechanical processing with a Energy supply is subjected, which the pulp in the form of mechanical splitting and fibrillation one Energy consumption of at least 20, preferably at least 30 and expediently at least 50 KWh per ton of fiber in one corresponds to alkaline aqueous solution, which has OH-bearing cations in the concentration mentioned, after which the

909842 / 07S1

- 13 -

Pulp is washed and neutralized. The upper limit for the expenditure of mechanical energy is on Estimated 200 Kwh, preferably not more than 150 Kwh and preferably not more than 125 Kwh per ton of fiber.

According to one embodiment of the production method according to the invention for the pulp that was used during tests carried out, the mechanical Processing carried out completely without external heat supply, with the supplied alkaline solution at room temperature is cooled.

According to a second conceivable embodiment of the method, which may be particularly useful in practice, this is Processing carried out in the form of a modified cold alkaline digestion, which in this description is called warm alkaline Splitting is referred to, which means that an alkaline solution is used when it is introduced into the processing device has a temperature between 40 and 70 ° C.

According to a further conceivable further development of the invention In the process, the fiber concentrations and the degree of mechanical processing are further closely related adapted in such a way that the temperature rise during processing is a maximum of 25 ° C, preferably a maximum of 15 ° C.

According to a second conceivable embodiment of the manufacturing method a relatively high fiber concentration is selected for the new fiber material and at the same time a relatively high energy expenditure in the form of mechanical processing energy such that it finally reached Temperature of the liquid discharged from the device

909842/0761 - 14 -

reaches the range between 90 and 130 ° C, corresponding to a temperature rise between 40 and 100 ⁰ C.

It is also the aim of the invention to offer a new paper with low air resistance, high opacity and good quality Retention capacity for fillers. According to the invention can. The new paper will be made by using a pulp is assumed, which has been produced in the manner described above, after which the pulp is beaten in this way becomes, as is customary with the use of conventional, essentially flax and / or hemp-based fibers, after which paper is formed in a manner known per se in a paper machine and wherein the fibers of the supply consist at least partially of the new fiber material according to the invention. In the case when the paper is for cigarettes is used, fillers such as limestone and / or other additives to pulp are also added prior to paper formation. Because of the splitting by cold alkali, i.e. the mechanical processing in a strong cold alkaline aqueous solution, it is possible to increase the opacity of the new paper with a degree of cleavage that is surprising is because pulp whipping tends to decrease opacity. With the new label of a paper according to According to the invention, this can be used positively as cigarette paper. A surprising result is also regarding of the air resistance of the new paper. Due to the mechanical processing according to the invention in a strong cold or "warm" alkaline aqueous solution, the air resistance is reduced, which means that the porosity increases with the degree of processing, which differs from previous experience with beating of Alfa pulp. The mechanism that could explain these new results is not fully understood.

809842/075 "

- 15 -

One can assume, however, that it is essential that the Fiber contains hemi-cellulose, which during processing is solved such that it does so in one way or another with the desired splitting operation works together, which is gentle on the fibers, which, for example, causes the fibers to only partially split and possibly also partially fibrillated, essentially without cutting. After the mechanical Processing the pulp is washed, whereby the dissolved hemi-cellulose is removed. By splitting also becomes achieves a paper that has a good holding capacity. The cold or "warm" splitting also creates the Paper-making final hitting effort decreased, which is a relative increase the opacity implies compared to the beating of common fibers which require more thorough processing. It is of course possible to use the pulp produced according to the invention with conventional pulp which is used for Cigarette paper is used or with other additives in connection with the use of pulp for manufacture of cigarette papers to mix. Such additives can, for example, limestone (calcium carbonate agent, which promote combustion, etc. in a known manner.

The new fiber material according to the invention can thereby be characterized that it consists essentially of fibers, obtained from wood, the majority of the fibers of the pulp consisting of a main trunk bent several times, along the length of which branches are arranged, which consist of fibril bundles, that the length distribution of the fibers after beating to 80 SR (Shopper-Riegler) is such that at least 25% by weight of the fibers do not pass through a sieve

§09842 / 0711 _ ₁₆ _

The number of meshes is 50 (mesh size 0.297 mm) and that the majority of the fibers have a width between 5 and 50 μm. Preferably at least 50% by weight of the fibers do not pass through a 50 mesh sieve and at least 30% by weight through a 30 mesh sieve (sieve opening 0.59 mm). Furthermore, a majority of the fibers have a width between 5 and 25 μm. Another characteristic feature is that the R ^ g value of the pulp is not less than 90 % . A paper that is made exclusively from this fiber material is ± if it has a weight of about 30 g / m 2, will have an air resistance between -1.0 and +2.0 log. Gurley, as well as a capillary climbing ability of at least 20 mm / 10 min., A tear length of at least 3 km and an opacity of at least 40 %, cigarette paper with a weight of 15 to 25 g / m and a filler content of 15 to 40 % CaCO produced. The paper can also contain fibers other than those from the new pulp. However, preferably at least 25 % of the fibers consist of fibers from the new pulp.

The invention is illustrated below by the description of tests carried out. In the description reference is made to the drawings, where:

1 shows the air permeability in the form of a diagram, FIG. 2 shows the machinability

3 shows the capillary climbing ability, Fig. 4 the opacity and

5 shows the tear factor as a function of the tear length for fibrous materials made of wood, which are produced in various ways have been treated according to the invention as well as for a number of comparative pulps made from Flax pulp and Alfa pulp are made up.

Ö09842 / 076 "i ORIGINAL INSPECTED

Fig. 6 shows the fiber length distribution at various Fibrous materials,

Fig. 7 is a photomicrograph showing the structure of Flax fiber material explains

Fig. 8 is a photomicrograph showing the structure of Wood sulphate pulp explains

Fig. 9 is a photomicrograph showing the structure of the fiber material produced according to the invention explained and

Fig. 10 is a photomicrograph showing a cigarette paper represents according to an embodiment of the invention.

The starting material used for the experiments was a sulphate pulp made from a mixture of wood from Nordic pine (Pinus silvestris) and spruce (Picea sfcbies) with smaller quantities (less than 15 %) birch (Betula verrucosa). The pulp was bleached with a conventional bleaching process based on chlorine to a brightness of 90 % according to the measurement according to SCAN-C 25:76. The viscosity was 45 m Pa / s (corresponding to 45 cP).

A VALLEY impact device was used in Examples 1-17 below. The amount of fiber in each example was about 450 g. The pulp in Examples 1-5 and 8-17 consisted of the above starting material, which was incorporated into the Valley impact device was filled in without further pre-treatment. The aqueous liquid contained in the added alkali

- 18 909842/0751

Sodium hydroxide in varying concentrations between 40 and 96 g / l. The pulp was in the Valley impact device processed under different loads and different fiber concentrations. The relatively small one Fiber concentration was based on the Valley impact device's limitations in this regard. Continued Tests carried out with equipment for technical production indicated that more concentrated Fiber blends are preferred. The loads selected were standard loads for sulphite and sulphate pulp in the Valley impact device. Examples were taken from the device after different processing times. In Examples 8-17 the "equivalent" energy consumption was calculated which is empirically known it is required during full operation in a production facility. The equivalent energy consumption is with the expression

E = 10 Y,

calculated, where

E is the energy consumption in KWh / per ton of pulp,

X is the percentage by weight of fibers in the suspension

and
Y means the processing time in minutes.

909842/075 "

- 19 -

The temperature of the supplied slurry in Examples 8 to 17 was about 20 ⁰ C and the discharged suspension is about 30 ° C.

After processing in the Valley impact device, the pulp was washed and neutralized with SOp water. The samples were then centrifuged to 30% dry weight. The R ₁₈ value for this fiber was measured according to SCAN-C 2: 61. New samples were taken from the pulp and beaten at 10% dry matter according to the usual operation in a PFI impact device to different degrees of impact, whereby different resistance to drainage was caused on the wire screen, which ^{can be expressed in 0} SR (Shopper-Riegler). A series of paper sheets were produced from this supply in a standardized Wennberg paper machine for nominal paper weights of 30 g / m 2. However, because of a certain amount of fiber which passed through the wire screen, the finished sheets only had a weight of about 28 g / m 2. The paper samples were subjected to a series of tests with regard to tensile strength (tear length), air resistance (time in seconds that are required for 100 cm ^{5 of} air to pass through a round paper

area of 645 mm passes under certain conditions, which are also called log. Gurley), capillary climbing ability (height up to which a liquid is absorbed in a vertical paper strip, the lower end of which is immersed in the liquid) and opacity (SCAN-P 8 j 75).

Example 1 (sample .. 77 B1. 21.1)

The pulp was processed in a Valley impact device under the following conditions:

S09842 / 07S1

- 20 -

Fiber concentration in the Valley impact device: 2 % alkali concentration in the Valley impact device: 60.0 g NaOH / l. Processing time in the Valley impact device: 30 minutes. Load: 6.792 kg.
R ₁₈ value: 90.9 %

The following values were measured on the paper sheets made from the basin pulp treated in the Valley impact device were manufactured:

SR ⁰ paper Tear-resistant air capillary Ops Table I. weight speed contrary Climbable ity 3 impact device, was standing speed (H) (XJ Revolutions 32 g / m ² Tear length log. mm / 5 min mm / 10 min % (W) 37 (L) in km Gurley PFI 42 67 28.7 2.8 0.11 36 45 59 0 27.7 3.1 0.18 37 46 60 500 29.6 3.8 ■ 0.85 23 30 61 1000 6000

Example 2 (sample 77 B1.22.1)

Fiber concentration in the Valley impact device: 2 % alkali concentration in the Valley impact device: 80.2 g NaOH / l.

909842/075 *

iNSPECTED

- 21 -

Processing time in the Valley impact device: 30 minutes Load: 6.792 kg R _i8 value: CZ 93 %.

The following values were measured for manufactured paper sheets:

Tabel SR ° II Tear-resistant Air- "' capillary Grandpa ag device, speed contrary Climbable ity honors weight was standing speed (H) (X) \'O 20th Tear length log. mm / 5 min mm / 10 min % FI 41 g / m ² (L) in km Gurley 53 1.6 -0.70 70 90 62 DO 30.6 3.0 -0.22 42 54 58 DO 29.0 3.5 0.18 28 35 59 DO 29.0

Example 3 (sample 77 B1.28.1)

Fiber concentration in the Valley impact device: 2 % alkali concentration in the Valley impact device: 80 g NaOH / l Processing time in the Valley impact device: 30 minutes Load: 4.982 kg R ₁₈ value: C ^ 93 %

909842/075 'COPY

- 22 -

The following values were measured for produced paper sheets.

Table III

Impact device,

Revolutions

PFI

Paper- Tear- Air- Capillary Weight Strength Resistant- Climbable-SR steadiness (H)

Opacity (X)

g / m tear length log. mm / 5 min mm / 10 min % (L) in km Gurley

750 21st 30.3 2.3 -0.62 54 70 57 5000 38 29.8 3.3 -0.12 36 47 55 15000 69 29.5 4.0 0.54 36 46 54

Example 4 (sample 77 B1 19.1)

Fiber concentration in the Valley impact device: 2% _t alkali concentration in the Valley impact device: 95.9gNaOH / l, processing time in the Valley impact device: 30 minutes, load: 6.792 kg
R ₁₈ value: 95.7%

The following values were measured for the paper sheets produced.

909842/075 '

- 23 -

Table IV

Impact device, revolutions, (W)

Paper- Tear- Air- Capillary Weight Strength Resistant- Climbable-SR ° steadiness (H)

Opacity (X)

PFI

g / m tear length log. mm / 5 min mm / 10 min % (L) in km Gurley

0 27 28.3 1 , 4 -0.70 67 81 65 1000 34 27.4 1 , 5 -0.60 59 74 64 2000 37 26.4 1 ,8th -0.60 45 53 63 5000 44

Example 5

Fiber concentration in the Valley impact device: 2 %, alkali concentration in the Valley impact device: 95.9 g NaOH / l, processing time in the Valley impact device: 10 minutes, load: 6.792 kg, cd 96 %.

- 24 -

9098A2 / 07

The following values were measured for the paper sheets produced:

Table V

Impact device,
Revolutions
(W) 0 SR ⁰ paper
weight Tear-resistant
speed air
contrary
was standing capillary
Climbable
speed (H) mm / 10 Opazi
activity
(X) PFI 2000 g / m ² Tear length
(L) in km log.
Gurley mm / 5 min. min. % 9000 9 95 18000 16 28.0 1.4 -1.00 77 68 55 26th 28.0 2.8 -0.70 55 43 56 53 27.4 3.2 -0.35 33 58

Example 6 (sample F1795)

This example as comparative example 1 relates to the production of paper from flax pulp. The R ₁₈ value of the flax pulp was 95.3%. The flax pulp was processed in a manner analogous to the wood pulp according to Examples 1 to 5 in a PFI impact device to different degrees of processing. The following values were measured for the paper made from this flax pulp.

909842/0751

- 25 -

Table VI

Impact device, revolutions (W)

SR

Paper Tear Resistance Air Capillary Weight Resistance Resistance to Climbing speed (H)

Opacity (X)

PFI

g / m tear length log. mm / 5 min. mm / 10 min. % (L) in km Gurley

* 0 42 24.5 2.6 -0.40 58 72 61 600 49 28.3 3.3 -0.05 51 62 66 2000 66 29.5 3.6 0.26 48 59 67 2500 71 28.8 3.5 0.34 33 41 68

* The fibrous material stuck to the propeller while stirring during the manufacture of the paper sheet.

Example 7

This example represents a comparative example 2 and concerns the production of paper from alfa pulp,

€ ± 97.5 % * The following values were measured:

- 26 -

0 9842/07 6 «■

Table VH

Impact device, paper tear-proof capillary O]

Revolutions weight air climbing ability

(W) SR ° resistance (H) S

was standing

PFI g / m tear length log. mm / 5 min. mm / 10 min.

(L) in km Gurley

"14 29.5 <■ 0.1 <.- 1
45000 80 26.5 4.8 2.6 15

Example 8 (Sample 77 B1, 62.5, Impact Operation No. 107/77)

Fiber concentration in the Valley impact device: 3.5 %,
Alkali concentration in the Valley impact device: 62.3 g NaOH / 1,
Processing time in the Valley impact device: 30 minutes,
Equivalent energy consumption: about 90 KWh / ton of pulp: ^. 93 %.

The following values were measured for the paper sheets produced:

- 27 909842/075 ·.

■ - COPY.

belle VIII SR ° Paper
weight Tensile strength
speed hitting device,
rotations
(W) g / m ² ' Tear length
(L) in km PFI

Tear resistance - Chap. Opacity air- climb- act resistant- (X) standing

Tear factor log. mm / 10 min. (Z) Gurley

2500 7000 0000

26.0 29.6

51.5 29.3 58.0 28.6

3.7 4.4 4.3

162 150 147

-0.40 49 50 0.18 34 46 0.30 36 46

Beis-Diel 9 (sample 77 B1, 62.3, impact operation no. 3/78 )

Fiber concentration in the Valley impact device: 3.5 %,
Alkali concentration in the Valley impact device: 62.3 g NaOH / l Processing time in the Valley impact device: 60 minutes,
Equivalent energy consumption: approx. 180 Ktfh / ton of fiber R ^ g value: approx. - ■ 93 %

The following values were measured for produced paper sheets:

- 28 -

09842/07 5
COPY

[Table IX

- 28 -

Impact device,
Revolutions
(W)

SiT

Paper tensile strength air cap.

rapier _ability tear resistance

ability stood ability

speed

weight

opacity

PFI

g / m '

Tear length Tear factor sec. Log. mm / 10 min. % (L) in km (Z) Gurley

5000 52 5 30th , 2 4, 4th 172 7000 56 30th , 2 4, 3 159 9000 67, 30th , 0 4, 6th 166

2.8 0.45 47
2.4 0.38 36

3.9 0.59 30

Example 10 (sample 77 B1. 65.3. Impact operation no. 10/78)

Fiber concentration in the Valley impact device: 4.0 % alkali concentration in the Valley impact device: 63.3 g NaOH / l, processing time in the Valley impact device: 30 minutes, equivalent energy consumption: 75 KWh / ton of fiber R ₁₈ - ¥ ert: ^ 93% .

The following values were obtained for the manufactured paper sheets measured:

909842/075 '

- 29 -

Table X

Impact device, turns

Paper- tensile strength- tear strength- air- cap. Opa weight resistance resistance

standing ability (X)

PFI

g / m tear length tear factor log, mm / 10 min. (L) in km (Z) Gurley

9000 49.5 28.6 4.8 154 0.16 28 44 13000 69.0 28.0 4.9 132 0.60 22nd 44

Example 11 (sample 77 B1.63.3, impact operation no. 2/78)

Fiber concentration in the Valley impact device: 4.0 % alkali concentration in the Valley impact device: 63.3 g NaOH / l, processing time in the Valley impact device: 75 minutes, equivalent energy consumption: approx. 185 KWh / ton of fiber R ₁₈ - ¥ ert: ^ 93 %,

The following values were obtained for the manufactured paper sheets measured:

909842 / 07S ^

- 30 -

Table XI SR ° paper
weight Tensile strength
speed Tear-resistant
speed • capillary
Climb
capability Grandpa
ta
(X Impact device,
Revolutions
on g / m ² Tear length
(L) in km Tear factor
(Z) air
contrary
was standing mm / 10 min. PFI 48.5 29.9 4.1 160 log.
Gurley 40 5 < 3000 63 29.3 4.4 150 0.28 24 5000 0.72

Example 12 (Sample 77 B1, 65.5, Impact Operation No. 1/78)

Fiber concentration in the Valley impact device: 5.0% alkali concentration in the Valley-Sr, impact device: 65.3 g NaOH / l, processing time in the Valley impact device: 75 minutes Equivalent energy consumption: about 150 KWh / ton of fibrous material R ₁₈ value: about < =: 93 %.

The following values were measured for produced paper sheets:

909842/075 '- 31 -

CXDPY.
ORiGiNAL INSPECTED

Cabelle XII SR ° paper Tensile strength Tear-resistant air capillary Grandpa: Impact device, weight speed speed contrary Climb did Revolutions was standing capability (X (W) 40 g / m ^Z Tear length Tear factor log. PFI 62 (L) in km (Z) Gurley mm / 10 min. Sä 30.0 4.2 177 0.01 37 4th 5000 28.6 4.4 154. 0.11 36 4th 9000

Example 13 (sample 77 B1 ♦ 66.3, impact operation no. 4/78)

Fiber concentration in the Valley impact device: 5.5% alkali concentration in the Valley impact device: 66.3 g NaOH / L, processing time in the Valley impact device: 78 minutes, equivalent energy consumption: 140 KWh / ton of fiber, R ₁₈ value: about Cz 93 %.

The following values were measured for produced paper sheets:

909842 / 075-!
-. COPY
ORIGINAL INSPECTED

- 32 -

Table XIII

Shock device, (W)

SR

Paper tensile strength air

importance of tear resistance

stand

Cape. Opazi-climbing ability- (X) ability

PFI

g / m tear length tear factor log. mm / 10 min. (L) in km (Z) Gurley

7000 51 34.5 4.4 178 0.41 30th 4S 10,000 65 29.3 4.6 150 0.64 28 ki

Example 14 (Sample 77 B1, 66.3. Striking operation No. 7/78)

Fiber concentration in the Valley impact device: 5.5 %, alkali concentration in the Valley impact device: 66.3 g NaOH / l, processing time in the Valley impact device: 95 minutes, equivalent energy consumption: about 175 KWh / ton of fiber R ₁₈ -value: about- ^ 93%.

The following values were measured for produced paper sheets: "

9098.4-2 / 07 5 * GOPY

ORIGiNAL INSPECTED

- 33 -

abelle XIV

storage device,
twists
(W) SR ° paper
weight Tensile strength
speed Tear-resistant
speed air
contrary
was standing Cape.
Climb
able to
speed (^ t) Grandpa
ity
(X) PFI g / m ² Tear length
(L) in km Tear factor
(Z) log.
Gurley mm / 10 min « 5000 50 30.2 4.4 172 0.40 29 41 9000 65 29.3 4.7 150 0.73 25th 45

Example 15 (Sample 78 B1, 02.3, Impact Operation No. 6/78)

Fiber concentration in the Valley impact device: 5.0% alkali concentration in the Valley impact device; 52.0 g NaOH / l, processing time in the Valley impact device: 85 minutes, equivalent energy consumption: 170 KWh / ton of fiber R ₈ - ¥ ert: <^ 92 %.

In this case, the mechanical processing could not be carried out using the -Valley impact device alone « It was necessary to use another auxiliary propeller.

- 34 -

909842 / 075-;
CXDPY

ORIQlMAL INSPECTED

The following values were measured for produced paper sheets:

■ Table XV

Impact device, paper, tensile strength, tear strength, air capillary Op

Revolutions weight resistance resistance increase zi

(W)

SR

steadfastness (H) te

PFI 59 , 0 g / m 2 Tear length Tear factor log, mm / 10 min. 70 , 0 (L) in km (Z) Gurley 3000 29 , 3 5.0 167 0.47 26th 7000 28 , 3 5.2 155 0.77 22nd

Example 16 (sample 78 B1, 02.3 »impact operation no. 5/78)

Fiber concentration in the Valley impact device: 5.0 % alkali concentration in the Valley impact device: 50.0% Processing time in the Valley impact device: 60 minutes Equivalent energy consumption: 120 KWh / ton of fiber, R ₁₈ - ¥ ert: <^

The following values were measured for produced paper sheets:

- 35 -

909842/07 5 '

COPY
ORIGINAL INSPECTED

Table XVI

Impact device, turns

(W) SR ⁰

PFI

Paper tensile strength tear strength air capillary opacity weight resistance increase did

standing ability (X)

g / m .. Tear length Tear factor log, mm / 10 min. - in km (L) (Z) Gurley

'7000 56 29.3 5.1 164 0.40 24 43 9000 64 29.9 5.0 147 0.81 24 44

Example 17 (sample 78 B1.09.3, impact operation Mr. 17/78)

Fiber concentration in the Valley impact device: 5.0 % alkali concentration in the Valley impact device: 40.0 g NaOH / l, processing time in the Valley impact device: 75 minutes Equivalent energy consumption: 150 KWh / ton of fiber R ₁₈ - ¥ ert:

91 %.

The pulp could even with an auxiliary propeller will not be further funded. It was therefore necessary to use hand-operated tools to help with the machining perform.

909842/075 1
MDOPY

INSPECTED-

- 36 -

The following values were measured for the paper sheets produced:

Table XVII

Impact device, turns

(W) SR ⁰

Paper tensile strength

Tear strength- air- capillary op- nity resist- Steig- zi

standing abilityytP (■

PFI 46 g / m 2 Tear length Tear factor log. mm / 10 min. 4; 59 (L) in km (Z) Gurley 4th 3000 29 , 6 5.3 162 0.45 27 5000 28 , 7 5.4 154 0.59 28

In Examples 18 to 20, a Bauer technical disk refiner was used for processing of the raw material, that made from wood Pulp, the pulp being of the same type as in the previous examples. The energy consumption per ton of pulp was calculated from the measured pulp flows and the electrical input Energy calculated. After being worked up in the disc refiner, the pulp underwent a treatment which corresponded to that of the preceding examples and in a PFI impact device up to treated to various degrees of degradation, after which sheets of paper were made and tested.

9098A2 / 075 '

COPY - 37 -

- .5 / -

Example 18 (sample B 70.6.100, impact operation No. 50/78)

Fiber concentration in the disc refiner: 6.0 % alkali concentration in the disc refiner: 70.0 g NaOH / l, energy consumption: 100 KWh / ton of pulp, R ₁₈ value: 93 %.

The following values were measured for produced paper sheets:

abelle XVIII
impact machine,
twists
(W) SR ⁰ paper
weight Tensile strength
speed Tear-resistant
speed air
contrary
was standing capillary
Climbing
abilitydi) Grandpa
ity
(X) PFI g / m ² Tear length
(L) in km Tear factor
(Z) log.
Gurley mm / 10 min. % 18,000
ί20000 60
76 28.0
28.3 4.4
4.6 106
93 0.34
0.95 24.
19th 46
46 Example 19 (sample 70.6.240, impact operation No. 49/78)

Fiber concentration in the disc refiner: 6.0 % alkali concentration in the disc refiner: 70.0 g NaOH / l

909842/075 '■

- 38 - COPY

ORlGiNAL INSPECTED

Energy consumption: 240 KV / h / ton of pulp,

The following values were measured for produced paper sheets:

Table XIX

Impact device,
Unidirectional
(W)

Paper, tensile strength, tear strength, air capillary Grandpa

weight resistance resistance increase rate

SR ° standing ability (H) (X

g / m tear length tear factor log. mm / 10 min, (L) in km (Z) Gurley

12000 29 28.3 4.2 159 -0.62 54 46 20000 64 27.3 4.4 120 0.03 37 44 25,000 78 27.1 4.7 94 0.81 27

Example 20 (Sample B 69.29.200, Impact Operation No. 46/78)

Fiber concentration in the disc refiner: 29 % alkali concentration in the disc refiner: 69 g NaOH / l, energy consumption: 200 KWh / ton of fibrous material R ₁₈ - ¥ ert:

93 %,

- 39

909842/075 ':

COPY

The following values were measured for produced paper sheets:

belle XX

impact device, rotations (W)

SfT

Paper tensile strength, tear strength, air capillary opaque weight, resistance to slope

standing ability (X)

PFI

■ 1

g / m tear length tear factor log. mm / 10 min. (L) in km (Z) Gurley

10,000 35 29.0 3.6 156 -0.63 68 47 18000 72 28.0 4.3 131 OiOi 40 47 20000 74 27.7 4.3 96 0> C6 48 25,000 81 26.7 4.6 107 0.57 30th 47 Example 21 (Sample F 50.30.50, Percussion surgery No. 29/78)

In this example a large-scale Frotapulper model R (Carlor & Sjögren or MoDoMekanf was used. The pulp was treated as follows:

Fiber concentration in the Frotapulper: 30 % alkali concentration in the Frotapulper: 50 g NaOH / 1 Energy consumption in the Frotapulper: 50 KWh / ton of fiber R ₁₈ - ¥ ert: Of 91

909842/075 ".
CXDPY

- 40 -

The behavior at higher energy consumption was also tested, up to 350 KWh / ton of pulp, which was possible. However, the temperature of the batch rose sharply and caused difficulties, because there were no suitable laboratory facilities to work up the treated pulp. However, in the case of large-scale technical conditions, these factors should not cause any difficulties. In this connection it should be noted that the rise in temperature in the suspension during mechanical working not only has disadvantages, provided that the pulp can be cooled quickly. Rather, the increased processing temperature and the increased plasticity of the fibers caused by the increased temperature appear to be responsible for at least some of the improvements achieved in the pulp properties and the paper made from the pulp. In the example, the temperature of the supplied mass was 20 ⁰ C and the suspension Austragetemperatur of about 50 ° C. When the energy supply was increased, the temperature increased accordingly to close to 100 C with an energy consumption of 350 KWh / ton of pulp. Therefore, according to a further embodiment of the invention, a high energy supply in the form of mechanical work is supplied in such a way that the temperature of the alkaline suspension discharged can be between 30 and 100 ^° C. and that the suspension is then quickly cooled for washing and subsequent aftertreatment.

Fibrous material processed according to Example 21 was aftertreated in the same way as in the previous examples. The following values were measured for the paper produced from this pulp.

909842/075 '- 41 -

COPY

hurry XXI SR ° paper Tensile strength Tear-resistant air capillary Grandpa lag device, weight speed speed contrary Climb ity rehungen was standing capability (X) (W) log. 47 g / m ² ■ Tear length Tear factor Gurley mm / 10 min. % PFI 76 (L) in km (Z) 0.13 29.7 4.8 114 0.74 33 45 3000 29.0 5.2 88 20th 42 3000

Example 22 (Sample F 1806, Impact Operation No. 78/77)

This example relates to the production of paper from flax pulp, the paper having a tear length in the of the same order of magnitude as the tear length of the paper according to Examples 8 to 21. Also made of this fiber Flax was processed up to in a PFI impact device different degrees of impact, after which a paper was produced which had the following properties.

909842/075
COPY

- 42-

Table XXII

Impact device, turns

(W) SR °

Paper tensile strength, tear strength, air capillary weight, resistance to rise capability

VALLEY (PFI) *

g / m - tear length tear factor log. mm / 10 min, (L) in km (Z) Gurley

15 (2300)

35 (4500)

60 (9GOOj

77.5 24.2 5.0

83.0 29.0 5.0

89.0 30.0 5.1

163

141

102

1.28

2.13

2.98

* The processing was done with the Valley impact device. The values in brackets have been converted to PFI.

Example 23

This example relates to the large-scale production of cigarette paper. Paper was made from a pulp consisting of a mixture of a pulp according to the invention, conventional sulphate pulp and a filler of pulverized limestone. 35 % of the bevel] in the batch was in the form of fiber material according to the invention from Example 21 (F. 50.30.50) and 65 % of the

909842/075

COPY

The fiber content was in the form of conventional sulphate pulp. The pulp contained 38 % limestone powder. The paper A produced was compared with a comparison cigarette paper B, in which the pulp according to the invention was replaced by an equal amount (35 %) of flax pulp. The following results were obtained.

ibelle XXlII

ipier weight Tear-resistant
speed air
contrary
was standing CaCO,
in the ^D
paper brightness ash
salary Opazi
ity (um-
reckon
on ρ23, C
g / no g / m ² Tear length
(L), km log.
Gurley Weight % Wt% Wt% * A.
B. 23.3
23.6 7.5.:
5.5 1.09
1.33 19
19 5 91
8 88 19.5
19.8 74.2
74.5

This example shows that a cigarette paper according to the invention has properties which are at least comparable to known cigarette paper which has flax fibers in the same amount as fibers according to the invention in the new cigarette paper. The air resistance is only log. Gurley 1.09, which means that the air resistance of a maximum of 1.2 log. Gurley can be expected when the fiber content of the cigarette paper with a weight of 15 to 25 g / m is at least in an amount of 25% by weight in the form of a cellulose pulp. 909842/075 1

- 44 -COPY ORIGINAL INSPECTED

discussion of the results

In the representations of FIGS. 1 to 5, the air resistance, the machinability, the capillary climbing ability, the opacity and the tear strength are shown graphically as functions of the tensile strength of the paper samples produced. In the diagrams, areas I to III show results with degrees of refinement R ₁₈ ^ 91 %, 93 % and 96 % with a pulp formulation with an? Aser concentration of 2 % according to the examples

I through 5 had been received. Area A explains paper made from Alfa pulp, Example 7. Area F 6 represents paper made from flax fiber material according to Example 6, the paper having a tear length of the order of 3 »5 km and area F 22 represents flax pulp paper made according to Example 22, the paper having a tear length on the order of 5 km. Areas I ¹ to III ¹ explain results which were obtained according to Examples 8 to 17. In particular, explains the area

I ^I results with a degree of refinement R ^ ₈ C? 91 % (example 17) »the area II ¹ results from the R ₁₈ - ¥ ert-92 % (examples 15 and 16) and the area III ¹ results from the R _1Q value ^ 93 % (examples 8 to 14). The triangles and line 20 illustrate results obtained when a disc refiner is used and a fiber concentration of about 30% by weight (Example 20) is used, while the circles and line 21 the corresponding result Tending to use a Frotapulper with approximately the same fiber concentration (Example 21).

- 45 9098A2 / 07 5 1

A number of conclusions can be drawn from the representations of FIGS. 1 to 5. Figure 1 shows that the air resistance for paper made of pulp, which has been beaten at a low fiber concentration, corresponds essentially to that of paper made of flax fiber, see. Areas I to III F 6. The illustration also shows that paper made of fiber, according to the invention has a high degree of refinement in terms of air resistance, can be significantly improved compared to Alfa cellulose paper with a degree of refinement R-, β'-2 =! 97.5 %. Figure 1 also shows that the air resistance of the paper can be improved if the pulp is beaten at a higher fiber concentration, which is important for cigarette paper.

FIG. 2 shows the revolutions PFI of the impact device for SR values that are extra-polished to 80 °. According to the illustration is achieved with a fiber material according to the invention a better whipping ability than with Alfa pulp. In spite of the considerably improved impact ability, the resistance to drainage is of the pulp according to the invention, however, and is very low in the undefeated (unprocessed) state in certain cases too low or even lower than is the case with alfa pulp, which in itself is surprising is essential in the large-scale production of the pulp in a factory. The diagram also shows that the whipping ability can be improved by increasing the fiber concentration.

Figure 3 indicates that the paper of the invention is a has better capillary climbing ability than paper made from alfa pulp and essentially at high levels of refinement has values that are just as high as those of flax paper Case is. The diagram also shows that the capillary rise

- 46 903842/075 ":

ability essentially by increasing the fiber concentration can be maintained in the blow operation and that the capillary rise is somewhat better than that of Flat paper of the same tear length is the case.

FIG. 4 shows that the opacity of the paper according to the invention has a value between that for paper made from alpha pulp and from flax fiber pulp. The opacity is somewhat impaired in the case of the paper which is made from pulp according to the invention which was whipped at a higher fiber concentration. However, the opacity is well over 40 %, which is satisfactory. It is also possible to improve the opacity by adding limestone powder to the pulp in accordance with normal practice.

Figure 5 shows that the tear strength is high and that by increasing the fiber concentration in the pulp during impact surgery can be improved.

It is also possible to deduce from the diagrams in FIGS. 1 to 5 that a striking device of the Frotapulpers type Making a better pulp for cigarette paper appears to be than a disc refiner. The diagrams also confirm the observation made at the outset that the quality of flax pulp is considerably between Different deliveries and even within the same delivery fluctuates, which is why the results with flax pulp are difficult to reproduce.

According to FIG. 6, the distribution of the fiber length in 4 different fiber materials is explained in the form of hestograms. The fibers that have been studied are those that have a fiber concentration of about 2 % (Examples 1 to 5)

- 47 909842/075:

have been processed, such as the pulp that was processed with a disc refiner at about 30 % fiber concentration (Example 20), a fiber that was processed with the help of a Frotapulpers at about 30 % fiber concentration (Example 21) and flax- Fibrous material according to column F. The columns shown furthest to the right in the histogram in FIG. 6 represent the amounts of fibers that do not pass through a 30 mesh sieve (sieve opening 0.59 mm). The one after that

■ The following columns show fractions that do not go / § ££ θ & the mesh count 50 (opening 0.297 mm), 100 (opening 0.149 mm) and 200 (opening 0.74 mm). Finally, the leftmost columns show fiber dust, i.e. the rest. The histograms clearly explain that the higher fiber concentration brings about a dramatic improvement in fiber length compared to the processing times at lower concentration such that the distribution of fiber lengths in the fiber, which was processed at a high concentration, essentially corresponds to that of flax pulp. This applies in particular to pulp that has been processed with the help of a Frotapulpers.

The diagrams in FIGS. 1 to 6 also prove the finding that can be derived from microphotographs, namely that the pulp according to the invention has properties which are similar to those of flax pulp. In particular a typical fiber of a pulp according to the invention has a structure which can be said to be a Combination of the favorable characteristics of wood pulp and Flax pulp is. Thus, the fibers of the fibrous material according to the invention have the main shape curved several times

- 48 -

909842/075:

Wood fibers taken over and at the same time the presence of fibril bundles taken from branching the original fibers grow out in a manner typical of flax pulp. According to their typical shape, there are thus the fibers of the fibrous material according to the invention from a main trunk bent several times, branches along its length consist of fiber bundles that are partially split off from the main stem. From the microphotographs it also follows that the fiber thickness corresponds essentially to the original wood pulp, which is a Means width between 10 and 100 μm, preferably between 15 and 60 μm.

In laboratory tests, paper sheets were produced with a weight of about 30 g / m 2. This weight is a common paper weight and the selection of this weight was made for experimental purposes only. In the preparation of of paper for cigarette production, the paper weight will be significantly lower or in the range from 15 to 25 g / m 2 as in Example 23. This reduced thickness of the paper naturally also reduces the air resistance of the paper according to known physical laws.

909842/075 '

e e r s e

11 e

Claims (26)

Claims 1. A method for producing a cellulosic pulp, thereby characterized in that a starting material which is im Cellulose - preferably consists essentially of / fiber material that / is made of wood was subjected to mechanical processing in a strongly alkaline aqueous solution, the solution being an aqueous one Is solution which has cations with OH groups in a concentration which, in the case of sodium hydroxide solution, 20 to 100 g, preferably Corresponds to 30 to 80 g NaOH per liter of solution. 2. The method according to claim 1, characterized in that the starting material consists essentially of a chemically, semi-chemically and / or thermomechanically obtained fiber material Wood consists and that the fiber a mechanical processing with an energy expenditure in the form of a mechanical Splitting and fibrillation of at least 20, preferably at least 30 and expediently at least 50 KWh / iEonne Subjected pulp in the alkaline aqueous solution and then the pulp is washed and neutralized to a pH between 5 and 10. 3. The method according to claim 1 or 2, characterized in that that the mechanical processing without external heat supply and with a cooling of the supplied alkaline solution Room temperature is carried out. §09842 / 075 ^ 4. The method according to claim 1 or 2, characterized in that the processing is carried out in the form of a modified cold alkaline cleavage, an alkaline solution is used which has a temperature between 40 and 70 ⁰ C when introduced into the processing device. 5. The method according to claims 1 to 3, characterized in that the concentration of the fibers and the supply of mechanical Energy are coordinated in such a way that the temperature rise during mechanical processing is a maximum of 25 ° C, preferably a maximum of 15 ° C. 6. The method according to claims 1 to 4, characterized in that the fiber concentration is so high and at the same time the energy input in the form of mechanical processing energy is so great that the final temperature of the discharged Liquid has a range between 90 and 130 ° C due to a temperature rise of the liquid between 40 and 100 ° C achieved. 7. The method according to claims 1 to 6, characterized in that the fiber material mechanically essentially without the preceding cold alkalinization is processed in such a way that the supplied pulp contains a substantial amount of hemi-celluloses which is dissolved in the aqueous alkaline solution during mechanical working. 8. The method according to claims 1 to 7, characterized in that the fiber material at a fiber concentration of at least 10% by weight, preferably at least 15% by weight and expediently at least 20 wt .-? £ is processed. §09842 / 075 '· -S- 9. The method according to claim 8, characterized in that the fiber material at a fiber concentration of 10 to 50 wt .-%, preferably between 15 and 40% by weight, suitably between 20 and 35 wt% is processed. 10. The method according to claims 8 and 9, characterized in that that the pulp is processed with kneading and / or scrubbing practically without cutting the fibers. 11. The method according to claim 10, characterized in that the pulp is processed in a device which is to the Group that consists of Frotapulpern, Frottatoren, Curlators and Frotapulpern. 12. The method according to claim 11, characterized in that the pulp is processed between cooperating screw flights will. 13. The method according to claims 1 to 12, characterized in that that the suspension discharged from the device is rapidly cooled. 14. A method for further processing the pulp which has been produced according to claims 1 to 13, too Paper, characterized in that the pulp is subjected to a further beating, after which the pulp in paper is made by a paper machine. 15. Fiber material, characterized in that it consists essentially of fibers which are obtained from wood, that the majority of the fibers of the fiber material consist of a multi-curved main stem, on the length of which branches are arranged, which consist of fibril bundles, that the length distribution of the fibers after beating 80 SR (Shopper-Riegler is such that at least 25 wt -.% of the fibers do not ^by §09842 / 0751 pass a 50 mesh sieve (sieve opening 0.297 mm) through it and that the majority of the fibers have a width between 10 and 100 µm. 16. Fibrous material according to claim 15, characterized in that the length distribution of the fibers after beating to 80 SR (Shopper-Riegler) is such that at least 50 wt .- ^ the Fibers will not pass through a 50 mesh sieve (sieve opening 0.297 mm) and that the majority of the fibers will be Have a width between 15 and 60 µm. 17. Fibrous material according to claim 16, characterized in that at least 60 wt .-% of the fibers after beating to 80 SR (Shopper-Riegler) do not pass through a 50 mesh sieve (sieve opening 0.297 mm) and at least 40 wt .-% of the fibers do not pass through a 30 mesh sieve (sieve opening 0.59 mm). 18. Fibrous material according to claims 15 to 17 »characterized in that it has an R ^ g value of not less than 90 % . 19. Paper, characterized in that it has been produced from a fiber material according to claims 15 to 18. 20. Paper, characterized in that it is made from a pulp with an R ₁₈ value of not less than 90 % , the pulp containing fibers made of wood, the majority of the fibers consist of a multi-bent main trunk, along which branches from Fibril bundles are arranged so that the paper has an air resistance between -1.0 and +2.0 log. Gurley owns that the paper has a tear length of S 0 9 8 4 2/0 7 B i - 6 - at least 3 km and an opacity of at least 40% with these values being based on standard laboratory Obtain paper sheets with a weight of about 30 g / m. it 21. Paper according to claim 20, characterized in that / a Weight of 15 to 25 g / m has that it 15 to 40 wt .-% Contains calcium carbonate and that it has a tear length of at least 4 km. 22. Paper according to claim 21, characterized in that at least 25% by weight of the paper fibers from the fibers made from wood with a main trunk bent several times consist, with branches of pibril bundles being arranged along the trunk length and the paper forming one. Air resistance of log. Gurley owns a maximum of 1.2. 23. Products, characterized in that they are made by means of paper according to claims 20-22. 24. Products according to claim 23, characterized in that they To represent cigarettes. 25. Cigarettes with a low tendency to tar formation due to the low air resistance of the cigarette paper and high brightness, characterized in that the cigarette paper consists of a paper which is made from a cellulose with an R ^ g value of not less than 90 % , that the paper has a weight of 15 to 25 g / m ² , that it contains 15 to 20% by weight of calcium carbonate, that it has a tear length of at least 4 km - 7 fi09842 / 075t -β- and that the paper contains wood fibers, these Fibers a multiple curved main stem and along this stem has branches from fibril bundles. 26. Cigarette according to claim 25, characterized in that at least 25 wt .-% of the paper fibers from the fibers with a multi-curved main stem and along this stem with branches consists of fibril bundles, wherein the fibers consist of the pulp which has been produced according to claims 1 to 14. S09842 / 07E1