DE28219C - Process for the production of cellulose and glycose from wood and other plant substances - Google Patents

Description

IMPERIAL

PATENT OFFICE

CLASS 55: Paper manufacture.

To carry out this process, the heartwood of the trunks of pulp and beef is carefully cleaned, split and, in the planing room A , cut into small and even slices using a planing machine.

Wood contains approx. 20 pCt. Water and, above all, the latter must be removed. This usually happens in the kiln BB ₁ below A.

The wood chips are brought through a trap door α onto the kiln horizons bb and, if there has been sufficiently pre-dried there, through the flap c into the actual kiln chamber B ₁ . The sole of the same consists of perforated iron plates.

Fresh air enters the space under the intestine through ducts e and is heated there by a system of pipes heated with condensation water. The hot air penetrates through the loose wood masses into the rooms Bi and B, where it dries the wood masses, and escapes with the water vapor through channels gg after the chimney.

If the wood is to be treated with alcohols later, z. For example, in the case of pine wood, the oil of turpentine contained in it must first of all be removed from it, which is achieved by distilling off at 160 ° C .; this is done by apparatus C located under the woodworking room.

In the middle of a chimney h the wooden discs are inserted through the manhole i into the iron cylinder equipped with a stirrer.

Give the upper half of it, and it circulates between the cylinder and the jacket when the oil of turpentine is distilled off with direct steam of 6 atmospheres of tension; for the subsequent drying of the wood, however, the very hot condensation water from the cooking coils, etc., is used. The steam or water enters through tap /, the outlet through tap m.

After the manhole and the taps η have been closed, the taps ο are opened until the necessary amount of steam has entered through the pipes //. These tubes lie flat against the cylinder, and the agitator causes the steam of 6 atmospheres flowing out of it to mix intimately with the wood and penetrate into it. Here the turpentine oil of the wood evaporates (boiling point 156.8 ° C.) and escapes with the water vapors through the helmet q, tap r and pipe s to the cooler /, where the turpentine oil and water vapors condense, and then through the collection u to flow to Bassin, S ^1.

The catchment u, as well as the catchments e _x and I ₁ mentioned below, are tightly closed vessels with a hemispherical glass bell. They serve as a regulator for the operator, since they allow him to recognize the course of the operation by the quantity and appearance of the distillate that is passing through the receiver.

If one sees that no more turpentine oil, but only water flows through the collection u,

the direct steam inflow to the jacket and the taps ο are shut off and the taps η and tap ν are opened. Fresh air will now flow in through the taps η and the flat pipes pp , which, with the help of the agitator, will come into contact with all the wood particles and, saturated with water, will escape through the tap ν and pipe w to the chimney. The cylinder is emptied through a narrow opening χ that can be closed by means of a slide. The small slide y is used to remove samples during the operation.

When the wood is dry, it is transported by elevator D to the first floor and, if necessary , is fed through the chimney a _L and a manhole into the wood burner £ , where the resin is to be removed from it.

Both hydrocarbons and alcohols can be used to dissolve the resin; but it is advisable to choose from these only those whose boiling point is as high as possible and whose price is at the same time as low as possible. These conditions are met from the hydrocarbons turpentine oil (boiling at 156.8 ⁰ C.) of the alcohols, particularly the fusel oil, a mixture of propyl, butyl and amyl alcohol; the latter is the main constituent of the fusel oil (boiling point of the fusel oil 128-132 ⁰ C, spec. weight 0.811).

The wood stove is BEZW _^2/3 with the very dry Holzspänehen and then the pump by means of a ₂ of the pumping station F of the basin G with turpentine. Fill the fusel oil so far that the liquid just covers the wood.

The cooking coil O ₁ fed with direct steam generates a temperature in the digester which is slightly higher than the boiling point of the extraction liquid in question, with excessive tension in the cylinder and the escape of the oil in vapor form through the condensation box C above the digester _{1 is} prevented. The oil vapor penetrates the pipes, which are surrounded by cold water, condenses and drips back into the wood mass, in order to dissolve new resin.

Any oil vapor still escaping from the condensation box is completely compressed in the cooler d _y and flows back into the basin G through the collecting egg. Goes to a lot of oil through the collecting _lt e so the temperature in the boiler by reducing the vapor inflow into the cooking snake O ₁ of the timber digester is lowered.

Is deposited in the wood tissue resin completely gone into solution, the pasty mass is by means of the tap /, ^ ₁ and of the tube in the Extractionscylinder H transferred.

A little above the bottom of this cylinder is a wire mesh covered sieve plate A ₁ through which the resin solution runs off. Anything that does not run out of the fabric by itself is forced out of the fabric by steam, which must have at least the temperature of the wood mass. When all the resin and oil have flowed out of the fabric and into the clarification basin J and only watery liquid flows through the sieve, which can be recognized by a sample from the small sample cooler i _x , the wood mass is still under the action of steam for some time respectively Exposed to water, as a result of which the extractives of the wood, which are soluble in the water, are also dissolved and flow off after the clarification basin J.

If the very hot resin solution gets into the clarification tank with steam water from the resin boiler, the oil and water vapors arising from the same would create a considerable tension in the clarification tank, if the vapors, _{captured by helmet z a} , could not escape to cooler k _2. From the latter they reach the collecting basin L.

In the clarification basin J the resin solution will be stored at the top and the water with the extractives at the bottom; The former, the level of which can be seen on the water level glass H ₁ , is drained into the suction pipe Vi _{1 by} opening the beaked cocks I ₁ above the watery layer and from there to the distillation apparatus K by pump d ₂ .

It consists of the cylinder O ₁ with the steam cooker P ₁ , helmet g _t , cooler S ₁ with cooling coil r, and the catch f _u from which the pure distillate flows back into the basin G. The residue in K, light-colored rosin, is drawn off at U ₁ and poured into molds.

The aqueous layer remaining in the clarification basin ^ / is drawn off at / ₂ ^{m from} the collecting basin L. In the extracts it contains mainly carbohydrates (possibly also some turpentine oil, if you have worked with it).

The collecting basin serves to completely separate the remaining oil from the watery layer. When this separation is complete, the oil is transferred through the cocks V ₁ and the pipe W ₁ into the basin G and the aqueous layer, to be later processed into glycose, to basin P and through the pump <r ₂ into the basin M promoted over the glycose cooker. The on

The cellulose remaining on the sieve Ji _{1 of} the extraction cylinder H still contains carbohydrates and salts which are insoluble in water; if pine wood has been processed, it also contains iron salts, which would later make the bleaching process very difficult. All of these substances are dissolved by dilute sulfuric acid. For this purpose the cellulose is withdrawn from the extraction cylinder H , carried to the first floor by means of the elevator N and poured into the glycose boiler O _{through the chimney tf 2} . The necessary amount of very dilute sulfuric acid is poured in through pipe P _{, whereupon the agitator 2 is set} in motion and so much steam is admitted into the space between the cylinder and the outer jacket m ₂ that the whole mixture boils gently. The agitator remains in constant motion for the entire duration of the operation.

This operation aims to remove the tissue as far as humanly possible from what is still there Clean incrustations, but in no case damage or damage the cellulose itself even dissolve, and the addition of acid must therefore be precisely controlled.

The time it takes to cook depends on the age of the wood. When the boil is sufficient, the cellulose is returned through pipe h ₂ to the extraction cylinder H , where the acidic liquid drains off and is passed through tap X ₁ into basin P. The cellulose is now washed out with steam until the draining water is acid-free, which in turn is tested _{by the cooler Z 1.}

The acidic liquid draining off contains significant amounts of glycose and is later used when boiling the glycose at the same time as the aqueous layer that remained under the resin solution, which is why it is also transported from basin P to basin M by pump C ₂ .

The cellulose is then ready. It either comes as it is to the bleaching room, or it is priced out and dried.

All cooling devices are from a high water reservoir JR. fed and the latter itself from the pump £ ₂ .

For certain types of paper you can very well use cellulose, some not of that kind of high purity, such as that obtained by the method outlined above. Such Inferior cellulose should be represented in the following way.

The wood freed from bark, pith, etc. is transformed in the planing room A into extremely fine chips, which, without further preparation , are carried directly into the extraction cylinder H , which is also provided with a manhole at the top for this purpose. After the cylinder is closed, high-pressure steam (of about 8 atmospheres overpressure) is passed into the apparatus from above and pressed through the chips, avoiding any boiling.

Due to the high temperature of the steam existing turpentine (at 156.8 ⁰ C.) is volatile, while the resin which melts at 135 ⁰ C., this is very thin. The steam seeks to penetrate the walls of the chips and ripens the resin, oil and other substances that can be removed by steam from such high tension with it to the clarification tank J, in which the resin or resin is contained. the non-volatile substances remain, while the greater part of the water and oil vapors in the collecting basin L condenses. After completion of the process, the steam is turned off, the mass of the Extractionscylinder H removed and direct the Glycosekocher O managed in which it with water to which has been added a little sulfuric acid described at about 130 ⁰ C. in exactly the same way as before , is freed from carbohydrates, iron, etc.

In order to make the greatest possible use of the steam used here, a number of extraction cylinders H are set up next to one another, so that the steam passes through them one after the other. The steam first reaches the extraction cylinder, which contains the most pre-cleaned wood mass. This cylinder bears the number 1 and the name Finisher, because in it the wood mass is cleaned as far as is possible with this process. The following cylinder, the content of which comes first in terms of purity to that of the finisher, has the number 2 and so on. The purity of the wood mass decreases with the height of the number and increases with the lower number. After Nq 1 has been emptied , Nq 2 becomes the finisher.

Each extraction cylinder H is provided with a miniature cooler i in order to be able to test the cooled distillate; each of these cylinders also has a storage space at its base, in which the heavy bezw. deposit as much of the impure parts as possible, while the steam freed from it, still capable of action, rises through a pipe located on the ceiling of the deposition room, from the first to the second, third, fourth, etc. to the last extraction cylinder, and from this finally, with Loaded with resin, oil and carbohydrates, it reaches the clarification basin J , in which the non-volatile substances settle. If there is no essential oil, the steam will be instantaneous

derived from J and used elsewhere without passing through Z; for this case J must be appropriately designed and equipped with a safety valve and manometer, while if essential oils are present in J the strained oil and water vapors located here, passing through the cooler K ₂ , reach the collecting basin L in order to condense the ethereal To effect oils.

Therefore, only one clarification and one collecting basin is required for this process to be.

The deposition space described above, located at the base of the extraction cylinder H , is provided at the very bottom with a tap or valve and a pipe, the latter being connected to / and L ; by opening the tap or valve from time to time, the heavier substances present in the storage space are diverted to / and L, depending on requirements.

As mentioned at the beginning, branches, bark, pulp etc. must be removed from the wood before it can be processed on cellulose. This waste, as well as needles, thin twigs, etc., are brought into the glycose cooker O in as finely chopped up as possible. If they contain essential oil in a worthwhile quantity, it is first distilled off through apparatus C.

As noted above, the Glycosekocher is a strong standing, an iron cylinder, which is up to _^3/4 of its height surrounded by an iron casing and provided with an agitator. The agitator shaft verticale c ₂ carries a plurality of arm systems, each consisting of three horizontal arms _o% of this agitator. O On these flat arms. ₂ O ₂ / are attached verticale rods Jr ₂ 2 which BEZW to the lower arm system to close. reach close to the bottom of the cooker. The rods p ₂ are arranged in such a way that no rod rotates around the shaft at the same distance as any rod of another arm of the same system. At their lower ends, these rods have paddles made of two triangular pieces of sheet metal that are riveted together with their longest sides perpendicular to each other. These paddles form open tetrahedra at the back and at the bottom, which mix the mass by furrowing through it like a snowplow. Moreover, one of the paddles is bent with the tip to the left, others with the tip to the right, so that one side surface becomes concave and the other convex, and one arm of a system only carries straight blades, another one curved to the right and the third one blades curved to the left. The agitator shaft also carries a long agitator arm s ₂ above these arm systems, which extends radially outward from the shaft and then extends tightly along the cylinder wall down to the bottom; it loosens the particles of the cooking substance hanging on the wall. This agitator sweeps every point inside the cylinder and incessantly tosses the mass through each other and thus mixes the poured liquid intimately with the wooden particles. The cock d ₂ serves for the direct supply of steam to the inner cylinder, e ₂ feeds the space between the cylinder and the jacket. The very wide water level glass f ₂ can be closed and the supply lines to the same can be cleaned with steam.

Only water vapors escape through helmet g ₂ , as the temperature in the stove cannot reach the boiling point of sulfuric acid. The glycose boiler, like all other apparatus and pipes which come into contact with acid or acidic water, is internally covered in all parts with a layer that cannot be attacked by sulfuric acid, e.g. B. with lead, and all closed vessels, in which hot substances come, are provided with safety valves, pressure gauges and thermometers. The glycose and wood stoves also have steam nozzles n ₂ to rinse out the cylinders after emptying. Except in the extraction cylinder, high pressure cannot be present in any apparatus because of the condensation apparatus that is installed everywhere.

The geschafften in Glycosekocher wood waste will have with dilute sulfuric acid and the contents of the basin M poured over, and this mixture, which is always the same Consistenzgrad there must, is boiled for constant stirring at about 130 ⁰ C. for several hours.

When the glycation process is complete, the mass is diluted with steam and water to such an extent that it can be transferred through pipe Ji ₂ to the extraction cylinder H. The glycose solution runs from H through tap Z ₁ to a vat Q.

The glycose still in the residue is removed by steam and water and also flows into the vat Q to be further processed afterwards. The residues in the extraction cylinder consist of undecomposed cellulose.

Claims (2)

Patent Claims: 1. The use of fusel oil to produce cellulose and glycose from wood and other plant products by boiling with steam as a heating medium. 2. The use of the devices listed below, which can be seen in the drawing: a) of the steam deoiling and dewatering apparatus C; b) the wood stove Έ; c) the extraction cylinder H; d) of the 'clarifying basin _ /; e) of the collecting basin Z; f) of the still K and g) the glycose boiler O in their combination and in the order listed for the purpose of illustration of cellulose and glycose from wood and other plant products. The use of a cylindrical boiler C equipped with a steam jacket, agitator and helmet for the purpose of de-oiling and draining wood and other plant products. The production of inferior cellulose from fine wood chips in extraction cylinders by means of high-tension water vapor. For this purpose I sheet drawings.