The invention concerns dispersion of cellulose fibres by strong mechanical agitation after addition of hydrocolloid and at solid conient up to 80%. This preparation results in a moulding composition, which is suitable for formation of cellulose containing fibre products.

By traditional production of paper and board, the raw material fibre is first dispersed in water in a mixer called pulper at very low solid content of only a few per cent. The rest, normally more than 95%, is water. Pulpers of special construction are described in the European patent applications 126.632 and 189.379. In these applications, pride is expressed of being able to work at solid contents a little above 20%.

In the paper industry it is generally accepted that the mentioned high amount of water is necessary for efficient treatment of the fibres to soften them, to make them expand, and thus to ease their dispersion with the aid of the pulper ^' s propeller.

The low solid content, which is used for traditional pulping of fibres and also for the very formation of paper, have made the paper industry utilise giant units which have to produce day and night the year around in order to pay the very high capital costs. The vast amount of water, has to be removed from the fibres afterwards. This results in environmental problems because of the high water usage, and most of all because part of the fibres and part of the employed additives run into the effluent as pollutants.

This invention solved these problems with a new method to disperse cellulose based fibres in water, which method comprises dispersion at solid content up to 80% after addition of one or more hydrocolloids during strong mechanical action.

Even though the inventor does not like to be bound to any theory for the mechanism being behind the invention, it is assumed that the hydrocolloid has a double function during the dispersion. It results in a high viscosity mixture, which is able to convey the forces from the agitator out to the individual fibres to tear them apart, and secondly there is a chemical affinity between the hydroxyl groups on the fibres and on the hydrocolloid so that the colloid penetrates in between the fibres, coats them and prevents them from reassociation.

The dispersion is done in a particularly strong mixer, preferably in a kneading machine which can be heated.

The invention is particularly intended as a preparatory step to new forming methods for paper and board, which are based on plastic forming by extrusion, injection moulding, coating, pressing or rolling. To get a good moulding composition for such use perfect dispersion of the fibres is not enough. It is also necessary to use so much hydrocolloid that the water is completely bound; more explicit that free water cannot be seen on the surface of the moulding paste, just after it has been pressed out through the die of an extruder. If free (glossy) water can be seen on the surface of the string coming

out of the die, it has been found in practice, that after only a short time the die is clogged by fibres, which have lost water and hydrocolloid. Complete water- binding is also an advantage for preparation of the moulding composition.

The moulding composition can be prepared at different temperatures. High temperature is particularly interesting, because it is then possible to disperse the fibres at still higher solid content than at ambient temperature. The upper limit for temperature is ca. 200 °C, as cellulose and hydrocolloid then start to discolour and decompose.

It has been shown that the moulding composition stands the high pressure which occurs during the kneading and in extruders by forming of the composition. Manufacturing of cellulose containing fibre products, according to this invention, may be simplified if separation of the fibres of the raw material and forming of the fibre products is done as an unbroken process, f.inst. so that the mixture is first kneaded at high temperature in the first part of a cook extruder and after that, possibly after cooling, it is formed by passing the die at the exit of the extruder or by being injected into a mould (injection moulding).

Fibres, which can be used with advantage, are fibres of cellulose, semi chemical pulp, groundwood or recirculated waste paper. Hydrocolloids, which may be used, are among others starch, starch derivative, dextrin, polyvinylalcohol, cellulose derivatives such as carboxymethylcellulose or hydroxyethylcellulose, animal protein like casein, vegetable protein f.inst.. from soya bean, vegetable gums like guar gum or locust bean gum, alginate, synthetic hydrocolloids as f.inst. polyacrylamide or flour from cereals like wheat, oat, rye, barley, rice etc., or from tubers as f.inst. potato or tapioca.

The amount of hydrocolloid needed for complete binding of the water depends on the water content of the mixture and still more on the water-binding efficiency of the colloid. With cheap hydrocolloid such as flour, the needed amount of colloid is about 4 - 20% of the amount of water, and with super efficient colloid like f.inst. polyacrylamide 0.4 - 2% of the water is sufficient.

It is particularly interesting to use cheap hydrocolloid, which has to be heated to gelatinise f.inst. a normal native starch. The starch may be added in ungelatinised form and brought to gelatinization after it has been mixed with the fibres and the water, by heat either supplied as such or liberated from the energy used for the kneading. When the starch gelatinises, this is clearly observed, as the mixture transforms from an inhomogeneous mixture to a homogeneous high viscosity paste; similar to a smooth dough.

Both dispersion of the fibres and forming of the fibre products is easiest carried out at a fair solid content of about 55%. However, after the forming there has to be a drying, and this is more elaborated at low solid content. It is therefore of advantage to perform the dispersion of the fibres at lower solid content than the forming.

As an example the dispersion of the fibres may be started by hot kneading at 40 % solid content. During this treatment water evaporates from the kneader, and the fibres get a perfect distribution when the solid content approaches 55%. The fibres are further worked up with heat supply in the kneader until the solid content reaches 75%. The subsequent forming needs somewhat higher pressure at 75% solids than at 55%, but this drawback and the inconvenience of the extra evaporation is more than counterbalanced by easier final drying. The hydrocolloids have a tendency to make the moulding composition sticky and may thus cause production problems. This stickiness may be reduced by adding processing aids such as wax and latex emulsions. The stickiness can also be reduced by increasing the solid content, f.inst. as described in the previous paragraph. In this way the moulding composition gets reduced adhesion to other objects and higher internal cohesion. Addition of wax with correctly chosen melting point may also increase the speed of forming, as the paste solidifies faster by cooling, f.inst. in an injection mould.

Below follows a description of some experiments, which were done to stipulate the conditions which are needed to obtain a moulding composition, which after compression to a thin sheet and careful examination appears perfectly homogeneous without occurrence of any fibre bundles.

The four first described experiments were done in a laboratory mixer of the type Brabender Plasti-Corder PI 2000. This is a mixer which gives a very strong kneading, and which may be heated. It is designed to imitate the agitation which takes place inside the extruders being used in the plastic industry. The mixer is composed of two thick paddles, which rotate with small distance to each other and to the walls of the chamber, much the same way as in a gear pump. The speed of rotation chosen for those experiments, which now are to be described, was 30 rpm. Mixer temperature was adjusted to 105 °C. Temperature of the mixture and the torque to the paddles were automatically recorded on a diagram. A pre-mix of 115 g unprinted newsprint paper moistened with 260 cc water was used for all the trials. These two basic components were mixed together in a domestic mix-master of the make Braun KM 32, and in which the mixing is done with a claw. This mixing was not sufficient to disintegrate the paper, so the pre-mix consisted of small pieces of paper soaked in water.

Experiment 1 was made for the sake of reference without hydrocolloid. The trial showed very clearly that the mixer did not succeed in transforming the mixture into a paste. Instead, the high forces in the mixer pressed water out of the mixture with such violence that water splashed out of the mixer. The torque quickly reached levels above 3 Nm, and it was impossible to obtain homogeneous distribution of the fibres.

Experiment 2 was done as Experiment 1 , however with the difference that 30 g maize starch was added to the pre-mix. The starch gelatinised quickly in the mixer, during which the mixture transformed to a paste, and the torque was

thereafter only 0.5 Nm. The kneading was continued for 7 minutes during which the solid content increased as a result of evaporation of water. After the 7 minutes the torque reached 3 Nm, and at the used rpm of 30, this is empirically known to be close to the maximum of which can be handled by injection moulding of plastic. The paste was taken out of the mixer, and it was found to be comparatively homogeneous, and the solid content was measured to be 45%.

Experiment 3 was done as Experiment 2, except for the difference that the amount of maize starch was doubled to 60 g. The behaviour of the mix was similar, but the paste became more sticky and had a tendency to stick to the walls of the mixing chamber. The torque was in the beginning 0.5 Nm and reached 3 Nm after 6 minutes . The mixer was stopped, and the sample taken out. It was perfectly homogeneous, and the solid content was 52%.

Experiment 4 was done as Experiment 3, but additionally to the 60 g maize starch 8 g stearic acid was also added. The stearin proved to give two advantages: The stickiness disappeared, and further it became possible to achieve a higher solid content before the torque reached 3 Nm. The last effect is probably because melted stearin improves flowability of the paste. The sample released steam in the mixer for the whole of 10 minutes, before the torque reached 3 Nm, and when the sample after that was taken out, it showed a solid content of 58%. Distribution of the fibres was perfect. Experiment 5 was done to establish the importance of strong kneading. Trial 4 was repeated, but in the domestic mix-master Braun KM 32 instead of in the Brabender mixer. The sample was alternately heated to 95 °C in a microwave oven and agitated in the mix-master. Even though this treatment was done in a fast sequence and repeated many times, it was impossible to achieve a homogeneous paste, so it is concluded that stronger mechanical agitation is necessary to perform the invention.

Trial 6 was done directly in a twin screw extruder intended for plastic and of the make Berstorf EO 7618/86. The mix was greater than for the trials described above, but the mixing ratio was about the same as for trials 4 and 5, namely 115 g unprinted newsprint paper moistened with 260 cc water and with addition of 60 g maize starch and 13 g stearic acid. The temperature in the extruder was adjusted to 95 °C. The extruder effectively transformed the inhomogeneous mixture into a homogeneous paste, which came out of the extruder die in the shape of a string with 1 mm diameter. Fibre distribution was perfect.

There was an evaporation of water from the hot string, after it left the die. By making the paste pass through the extruder many times, it was possible to increase the solid content to 80%, before at 95 °C the paste became so hard and brittle that it had lost its mouldability.