JPS58500901A - Textile material processing method and device - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] Textile material processing method and device The present invention provides an internal surface and/or an external surface, each of which constitutes a gap or a pore. Relating to a method of treating a material containing fibers having properties to impart desired properties to the fibers. Ru. Such fibers include natural fibers with internal cavities or pores, such as cellulose. fibers or wool fibers, or with internal cavities or interstices or pores as described above. There are man-made fibers that have an external surface portion that consists of: For example, such man-made fibers include For example, fibers with a cross section with protrusions forming spaces between each other, or fiber spaces in the material. Some have a spiral structure that forms .

Materials include wheat straw, wood waste or other wood materials, or composite paper or woven There are fibrous sheets or woven materials such as cloth or non-woven fibrous materials.

In the method of this invention, the material is heated and/or dried, and then the gap or consisting of compressing the material to an extent sufficient to at least partially compress the pores . In principle, compaction can be carried out by any method, for example hydraulic or mechanical compaction. This can be done by law. However, the gap or air gap composed of a single fiber To compress the pores and/or the gaps or pores that exist between the fibers, the material can be rolled. For example, by treating the entire fiber material roller with a suitable facing surface, At the same time, the roller and the opposing surface sound mutually with strong pressure through the gap formed between them. It is necessary to apply very high pressure to the fibers by pressing against them. The opposite surface is static. It may be in a flat state and may have a flat or curved surface. however Rolling involves passing the fibrous material through the nip of a pair of co-moving rollers. It is particularly preferable to do so. If the material contains natural fibers, the amount of natural fibers Preferably, the compression is sufficient to permanently deform at least some of the vesicle walls. .

straw, veneer, wood waste or other wood materials, or pulp, cardboard or The laminated paper is compressed or rolled at sufficiently high pressure under substantially dry conditions. In the case of fiber processing, the fibers are crushed to some extent, thereby increasing the SR' of the fibers. The treated material can be made into pulp without further processing. For the production of paper, paper, and the like, such as greaseproof paper, parchment paper, and the like. Make it as thin as possible.

In various known methods, such as rolling, cellulose fiber fabrics are roll compacted.

However, in such known methods, the pressure applied to the fibers is Using insufficient pressure to permanently deform the wall. In the method of this invention As such, the pressure applied to the fibers typically substantially permanently deforms the cell walls of the fibers. and is substantially higher than that of the seven known methods.

That is, in the method of this invention, the pressure in the gap between a pair of co-moving rollers is reduced. The force is typically substantially higher than 100 kp/Cr/L2 and 10,00 0 kp/m2, and the pressure is often 1000 kp/cm2. IQ, QQ between Q$’12, for example 2000kp/CrIL2 and 10 , 000k p7.2 or between 5000kp/crL2 and 1 0,000kp/m2.

In an important aspect of this invention, the Sometimes a liquid substance is supplied to the material. This liquid substance may contain, for example, the desired properties for the fibers. substances, such as impregnants or modifiers that impart desired properties to the fibers, or The combination of soaking agent and modifier may or may later substantially evaporate and cause slippage. There are liquid substances that function only as agents (see below).

The fibers are compressed or rolled in the presence of an effective amount of a liquid substance as described above. In this case, this substance acts as a lubricant, thus avoiding fiber fragmentation.

However, during rolling the fibers are compressed and flattened, which causes The gas, e.g. air, is expelled from the interstices or pores formed by the fibers and The fibers are surrounded by a film or medium of liquid material.

This compression or rolling process allows the dispersion of the liquid substance in the fibers and the separation of the single fibers and the liquid substance. Close contact occurs between Fibers have some resilience, so After compression or rolling, the flattened fibers are at least partially restored to their original shape. tend to return to the original shape, and thus the initial presence within and/or between the fibers Interstices and pores are partially reformed.

However, since the fibers are surrounded by a liquid substance, this substance can be sucked into the gaps. This further increases the contact surface between the liquid and the fibers.

One form of this invention can be considered as a continuous treatment of textile materials, in which The material is compressed under high pressure, and then the pressure is removed in the presence of a liquid substance, This results in a pressurized/vacuum effect, creating gaps within and/or between fibers. Alternatively, at least a portion of the pores are filled with a liquid substance.

Part of the energy supplied to the rollers is converted into heat in the roller gap. , and due to the temperature increase in this area, the temperature during roll processing increases. A chemical reaction between the liquid substance and the fibers is promoted. also by the roll processing itself. Chemical-physical changes occur in the amorphous structure of cellulose fibers, and this change involves cellulose It has been experimentally shown that this may involve the formation of hydrogen bridges in the amount of silver.

In embodiments of the invention in which the liquid is supplied prior to or in conjunction with compaction or rolling. Therefore, if textile materials are treated, some of the water present in the material can be removed even before the liquid is applied. or may interfere with sufficiently good contact or affinity between the fibers and the liquid substance. . Therefore, before and/or after compressing the fibrous material, a liquid substance (in which be as completely hydrated as possible prior to dispensing (which may contain water) It is necessary to remove. Such water (free water and bound to fibers) water) and possibly also to increase the temperature of the compression section. , applying the liquid substance and/or carrying out a heat treatment and/or compression treatment. Or carry out a drying process, preferably a strong drying process. For example, the theory of hydroxyl groups in textile materials when expressed as reactive cellulose hydroxyl groups relative to stoichiometry. The dry matter content of It is desirable to dry to a range of 99.999%.

The heating temperature should be within a range that does not cause damage or deterioration of the fiber material (and that does not cause damage or deterioration of the fiber material). It is preferable to select the highest possible temperature (as long as the water of crystallization present in the water is not lost). . When the fiber is cellulose fiber, the heating temperature of the fiber material is 100 to 275°C, especially 120 to 250°C, preferably about 160 to 220°C, more preferably 180°C ~200°C. This results in higher than 98%, preferably 99%, and In particular, the goal is to dry to a range of 99.1 to 99.999%. This drying It also destroys the monomolecular water layer bonded to the fiber surface and releases cellulose δ hydrocarbons. Making cellulose more reactive towards any substance that can react with xyl groups must be something that can be expected. Reaction between cellulose and added liquid substance Both when such a reaction is required and when such a reaction is not required, Heating the cellulose fibers is an essential feature; The lignin component softens, and this softening allows the liquid substance to penetrate into the fibers (using the liquid substance). ) and reduce the brittleness of the cellulose fibers, which reduces pressure It is believed that the risk of damage to the cellulose fibers during the shrinking process is reduced.

Cellulose is produced by heating to a somewhat higher temperature than 250°C under conditions of exposure to oxygen. is known to decompose. Therefore, cellulose fibers must be present at higher temperatures. It is necessary to perform heating in a clean atmosphere.

In the absence of oxygen, carbonization of cellulose fibers is prevented and cellulose The fibers can be heated to 250°C without any loss of crystallization water bound in its components. Can be dried at high temperatures.

Heating of the fiber material can be done by infrared irradiation, e.g. by infrared heating means, for treatment. By irradiating the supplied fiber material, high frequency treatment of the fiber material or in heated dry air or heated oxygen-free gases or gas mixtures. This can be done by passing the fibrous material through the material, or by a combination of these methods.

To compress the fibers, the fiber material is passed through the gap between a pair of compression rollers at an appropriate low speed. This can be done by forcing. Usually the rollers make up the roller nip Rotate the cylindrical surface of the roller so that it moves at the same speed and in the same direction. Ru. As an alternative to this method, the rollers can be It is also possible to rotate the rollers at different degrees, and the rollers can be rotated in opposite directions. You can also force it. The compression process applied to the fibrous material depends on the rotational speed of the rollers. , the diameter of the roller, and the thickness of the web or material layer fed into the roller nip. Depends on. To evenly and effectively compress all fibers in the fibrous material and/or or to provide a thick web or layer of material in the gap between the rollers. It is possible to pass through gaps between two or more pairs of rollers one after another. According to certain embodiments, one The two roller pairs in series are composed of three rollers, and one roller (intermediate roller) roller) in conjunction with the other two rollers, and each of the other two rollers Together they constitute a roller gap. A series of multiple pairs of rollers are used to move the material to be processed. The roller gap becomes smaller and smaller in the direction of the Gradually increase the force with which you press the Ra pair. Using multiple pairs of rollers The distribution of liquid substances in the fiber material is improved. 2 or more pairs of rollers If passed, liquid substances and/or other liquid or particulate additives, e.g. The material described can be fed between two adjacent pairs of rollers.

The liquid substance may be prepared in any suitable manner, such as by passing the material through a container of the liquid substance. In addition, it can be supplied to textile materials. However, one preferred embodiment , preferably by an airless atomization method, e.g. one or more The liquid substance is sprayed onto the fibrous substance by the nozzles. The liquid substance has dissolved or When containing suspended solids, the nozzle tends to become clogged. however 1 This can be done by feeding the liquid substance into the nozzle in a pulsating flow and or This can be prevented by heating the nozzle to a temperature where the liquid substance has the appropriate viscosity. can. (Also, heating of the liquid supply nozzle or any other liquid supply means is as follows. , generally required when the liquid is a melt). In another advantageous embodiment, e.g. For example, on a roller partially immersed in a liquid substance, from one surface of the roller. Add liquid substance. The liquid substance is applied to the textile material in a certain amount slightly in excess of the required amount. and drain excess liquid from the fibrous material after the material has passed through the first pair of rollers. Remove from. One method of applying a quantity of liquid substance to a textile material is, for example, by applying Apply liquid substance to one or both rollers by licator roller or spraying This is the way to do it.

As mentioned above, the temperature of the roller gap of one or more pairs of rollers is substantially increased. It is preferable to

This temperature is determined by heating at least one of the rollers used in roll processing. If the temperature rises further due to This prevents or avoids the adhesion of solidified substances to the roller surface. I can do it.

After compaction or rolling, the fiber material is further processed in a fiber crusher or fluffing device. Can be processed and crushed. The crushing equipment is a wet machine such as a pulp crusher. There are wet crushing devices and dry crushing or fluffing devices such as humer mills. fiber The material is high-pressure compacted or rolled as described above and then processed in a thermomill. When processed, produces a very homogeneous crushed product without forming lumps or fiber agglomerates. Obtainable. If desired, process with a -. Other liquid particles, sand, or grinding aids can be added to the fibers during the process. was discovered.

The fibrous material is compressed under dry conditions, i.e. with the addition of a solution lubricant, followed by Mechanical processing of the fibers is necessary when processing with the fluffing equipment of a fiber mill. Multi-fibers may deteriorate due to the temperature increase that occurs during processing. Fluffing textile materials A suitable lubricant, e.g. Add kerosene or ethanol (or any other liquid substance, e.g. impregnating agent) It has been found that in particular it is possible to control or even prevent said deterioration. . The ratio at which mechanical energy is converted to thermal energy by adding such a lubricant The lubricant also acts somewhat as a coolant. I will.

The invention further relates to an apparatus for use in carrying out the method as described above; is a roll means comprising at least one pair of rollers, a sheet or web of fibrous material; a supply means for supplying a reservoir into a roller gap constituted by a plurality of pairs of rollers, and heating and/or drying means of Gallo heat and/or drying pot of the supplied fiber material; consists of Preferably, the device further applies the fibrous material upstream of the rolling means. Means for applying a liquid substance or means for applying a liquid substance to a roll means , and crushing means, in particular means for dry crushing the fibrous material downstream of the roll means. , in particular -.

The invention further provides for a fibrous material having cell walls permanently deformed by compression. related.

The invention will be explained in more detail in conjunction with the drawings. In the drawings, Figure 1 is Fig. 2 shows a schematic diagram of a device for treating textile materials according to the invention of Figure 3 shows an enlarged view of the case in which the fibers are rolled with heavy roll pressure. This is a perspective view showing the device in great detail; Figure 4 shows an even smaller example of the device. Fig. 4a shows an outline of a modification of the apparatus shown in Fig. 4, and Fig. 5 shows a schematic diagram of a modification of the apparatus shown in Fig. 4. Third component of the sump apparatus for processing straw, wood chips and similar starting materials 6 is a side view schematically showing an example of a body, and FIG. 6 shows a number of flat members connected to each other. FIG. Figure 7 shows impregnating agent inside. Fig. 8 is a scanning electron micrograph of a treated fiber web with dispersed Figures 9 and 10 are scanning electron micrographs showing the properties of fibers produced according to this invention. shows a monofilament treated and subsequently extracted with dichloromethane; and Figures 11 and 12 are treated according to this invention and then dichloro Fibers extracted by methane (Figure 11) and unextracted fibers (Figure 12) ) are shown respectively.

FIG. 1 schematically represents an apparatus for processing fibrous cellulosic material in the form of a web 10. The web 10 is transferred from the supply roll 11 to the inside of the pair of high pressure rollers 12'. It is continuously fed to at least one roll device 12. fibrous web material It passes through a heating and drying device 13, which includes a supply roll 11 and a liquid supply device. The device 14 is arranged between a liquid storage container 15 and a spray nozzle li. The nozzle 16 is configured to heat the liquid substance contained in the storage container 15. and downstream of the drying device 13 and upstream of the roll device 12 the web material 10 It is arranged so that it is sprayed on. In the roll device 12, the fibrous web is , as shown in FIG. It is compressed under very high pressure, enough to cause it to shrink.

It is completely dried by the drying device 13 and then sprayed by the nozzle 16. The fibrous web moistened with the liquid material is transferred between the rollers 12'. As it passes through the gap between the fibers, the liquid substance comes into intimate contact with the entire surface area of each filament, and The excess liquid material 18 is continuously removed as shown in FIG.

Gas or air is forced as the fiber gap 17 is compressed in the roll nip. removed from the gap.

After the material passes through the roll nip, the resiliency of the fiber cell walls causes the nip to re-open. There is a tendency to form, whereby some of the liquid material is sucked into the interstices.

However, the roll pressure is so high that the cell walls are considerably deformed and the single fibers become fluffy. Therefore, the fibers passing through the roll device 12 do not completely maintain their original shape. Low compression/expansion effects applied to the fibers and the liquid substances applied to them during processing or Due to the pressure/vacuum effect, liquids can be applied over the entire internal and external surface area of the fibers. Close contact and uniform distribution of the materials occurs. Energy used to drive roller 12' During the rolling process, fibrous materials are exposed to high Warmth is applied and this, combined with the uniform dispersion of the liquid material, causes constitutes optimal conditions for physical and chemical reactions between fiber materials and liquid substances. . As explained below, liquid substances can be used, for example, to impart desired properties to fibrous materials. Any desired impregnating liquid material that can be applied can be used. This way After the fibrous web lO treated in this way leaves the roll device 12, this web is fed to a hammer mill 19 or other fluffing device in which the material is crushed and i If necessary, further processing can be carried out at the same time.

FIG. 3 shows the apparatus of FIG. 1 in greater detail. In this specific example , the heating and drying device 13 is configured so that the fibrous web 10 supplied from the supply roll 11 is It consists of a tunnel 20 that it passes through. While the web 10 passes through the tunnel 20, this The web is illuminated by a number of infrared radiation devices 21 located in the upper part of the tunnel. heated. The irradiation device 21 passes partly through another passage 23 in the upper part of the tunnel. A blower 22 blows out cold air, and some compressor with a drive motor. Cooling provided by suitable means such as a machine 24 and arranged in the irradiation device 21 It is cooled by pressurized air circulating through the passages. If desired, further web Heating can be applied from below or water vapor can be removed from below the web.

The web is completely dry and leaves the heating and drying device 13 under heated conditions. 10. passes under the spray nozzle 16. This nozzle 16 covers the entire width of the web 1°. It has a large number of nozzles to spray the liquid substance uniformly over the area, and , this nozzle is arranged so that the jet includes a velocity component in the direction of movement of the web 10. is preferred. The liquid substance is transferred from the liquid storage container 15 to the supply bonder 25 through the supply conduit. 26 to the nozzle 16. A liquid substance is solid or solid at room temperature. If the viscosity is too low, use a heating jacket containing an electric heating element. The tank surrounds each reservoir 15, and the liquid is passed from the reservoir 15 to the supply conduit 26 (this conduits are also supplied with electricity (which can be suitably enclosed by a thermal jacket). Ru. The liquid is passed through, for example, a hot melt type heating device 27, where it is further heated. be able to.

In the storage container 15, the heating device 27 and the supply conduit 26, the liquid substance is is pumped by the supply cylinder f25 and well distributed into the nozzle 16. furthermore, the liquid viscosity ensures sufficient penetration of the vaginal fluid into the fibrous material. It is heated like this. However, heating of liquid substances cannot be performed at any stage of the heating process. Excessive amounts that may cause decomposition, denaturation or undesired polymerization of the liquid material It is controlled so that it does not become a thing. stored in storage container 15 and heating device 27 pressurized to prevent the liquid material contained in it from being oxidized by contact with ambient air. Nitrogen or other inert gas is supplied from the stored gas container 28 to the storage container 15 and heating device 27. can supply the body. The liquid application device 14 includes a device for applying a liquid substance to a nozzle 16. A sump valve (not shown) may be included to control the intermittent supply. Ru. This valve and the supply pump 25 are operated by pressurized air generated by the compressor 24. and the intermittent supply of pressurized air to the valve is electrically controlled. This can be done using a solenoid valve. The liquid flowing through the spray nozzle thus generated It is possible to effectively prevent clogging of the nozzle orifice due to the pulsating flow of substances. Wear.

The web 10 sprayed with the liquid substance passes through a guide path between a pair of guide rollers 29. 30 to the roll device 12. This roll device 12 is shown in FIG. In the specific example, it consists of two separate roll units 12a and 12b. Ru. Each of these roll units consists of a pair of rollers 12', which It is rotatably attached to the arm (31) and is driven by a drive motor 32. be done. Each roll unit consists of equipment used, for example, in the production of gold leaf and other metal foils. The system is designed to be subjected to very high pressures in the nip, such as , and this roll pressure is adjusted by the manual handle 33. roll unit 1 The excess liquid substance separated from the 2a cylanib 10 is collected in the receiver 34. and is returned to heating device 27 through return conduit 35. Impregnated into web 1o In order to prevent adhesion between the liquid substance and the roller 12', and to prevent the fibrous nature of the liquid substance, In order to further improve the penetration and dispersion into the web lO, these rollers can be used, e.g. For example, directing a heated air stream towards the rollers and the web 10 passing between the rollers. Preferably, the heating is performed by a heating device 36 that can be used.

Although two consecutive roller units are shown in Figure 3, one roller unit or any number of consecutive roller units, thereby Increase the thickness of the web 10 and/or the speed at which the web 10 moves through the roller unit. can be reduced. Controlled speed for optimal treatment of fibers in the web Preferably, the web is moved through one or more roller units'. Yes. This speed depends, for example, on the thickness of the fibrous web, the number of roller units and the Depends on the diameter of the lar. For example, when the diameter of the roller is relatively large. The compression of the fibers is not rapid and therefore as the diameter of the roller increases. can increase the speed of web movement. In addition, a large number of roller units Its use improves the dispersion of liquid substances in the fibrous web 10. 2 When using more than one roller unit, the adjacent roller units.

In order to prevent tension sillage in the portions of the web 10 located between the adjacent In order to prevent excessive curves 37 from being formed in the web 10 between the units, It is necessary to strictly control the mutual rotation speed between units. first roller unit Since the length of web 10 increases while passing through port 12a, both units are identical. Even if the second roller unit 12b is driven at a slightly higher rotational speed, must move. This means that the drive motor is controlled by a transmission (not shown). This is achieved by adjusting the controller 32.

If desired, between the roller units 12a and 12b and/or between the roller units 12a and 12b. between the cut 12b and the spray mill 19, e.g. by means of an additional spray nozzle 38. , additional liquid or solid additives may be provided to the web 10.

Rolled and impregnated web 101d, 07-unit 12 It is transferred to the hammer mill 19 by a pair of transfer rollers 39 that are driven simultaneously with b. sent. Processed in a hammer mill 19 driven by an electric motor 4o A very large mechanical force is applied to the fibrous web, which causes the a male material to complete. Completely crushed. This crushing process is based on the amount of roll treatment applied to the fibers in the previous stage. highly encouraged. The heat generated in the hammer mill is quite large, so it is necessary to supply cooling air. In some cases, the temperature may be controlled.

- due to the high temperatures and large mechanical effects exerted on the fibrous material in the thermal mill 19. The physical and chemical reactions between the fibers and additives that started during rolling are completed. do. Additionally, additional additives, such as funnel 41 shown in dotted lines in FIG. Continuously fed powder can be fed directly to the hammer mill.

Such additional additives include any liquid substance that imparts desired properties to the fiber, e.g. Examples include lubricants such as kerosene or ethanol.

Figure 4 shows a specific example of a modified version of the device shown in Figure 3. Corresponding elements of the embodiments have the same reference numerals. In the specific example shown in Figure 4 In this case, the passage 20 of the heating and drying device 13 includes a plurality of vertically arranged sections 20 a, 20b.

and 20e, and at the ends of these parts the web 10 is It is guided by guide rods 51-53. Similarly, the liquid application device 14 and the roll device 12 , hammer mill 19, and filtration device 42 are arranged vertically.

FIG. 4a shows a specific example of the apparatus shown in FIG. 4 with modifications. In Figure 4a In this case, the liquid application device 14 is connected to an opposing portion of the cylindrical surface of the roller 12' with a suitable bond. It is replaced by a liquid container 66 contained in a container formed by a fixed end wall 67. Ru. The liquid level in container 66 is sensed by liquid level sensor 68 and the liquid is transferred to the liquid storage container. From the vessel 69 it is fed into the container 66 through an outlet pipe 70 having a valve 71. Control device 72, the liquid level in the container 66 is determined based on the signal received from the liquid level sensor 68. Valve 71 is controlled to be substantially constant. As schematically shown, the spring 73 1) The o-rollers 12' are pressed together with very strong force and the web 10 is as described above.

Although the embodiments shown in FIGS. 3 and 4 are applied to treating fibrous webs, The embodiment shown in Figure 5 is used to process wheat straw, wood chips, and other particulate materials. Ru. A starting material such as wheat straw is fed into a receiving funnel 54 from which the material is heated and heated. and a drying device 55, where the material is dried, for example by heated air. Ru. The heated and dried material falls from the dryer 55 into the funnel 56. During this period, a spray nozzle 57 is supplied with liquid from a storage container 58 by a pump 59. A liquid substance can be applied to the material. The moistened material is transferred from the funnel 56 to the The cellulose material is supplied to a roller device 60 of various types, and then the cellulose material is rolled. Excess liquid separated from the cellulose material as it passes through the cellulose device 60 is returned to the cellulose material. The pipe 61 is completely passed through and returned to the storage container 58.

The material passed through the roller device 60 is then passed through the mill 62 or other fluffing device. Fallen and crushed fibers are produced from these devices similar to those described in connection with Figure 3. is introduced into a filtration device 63 of the type.

The fibrous web 10 treated by the apparatus or equipment shown in FIGS. 3 and 4 is elastic. It is a highly porous material with strong properties. However, the method of this invention For use with wood or sheet materials, such as relatively rigid wood sheet materials. Can also be done.

In this case, the roller 6 In order to prevent separation in the roller gap of 5, the Sheet materials or panels can be constructed from joined sheet elements (such The V-joint type is also suitable for joining sheets of resilient material).

Such panels can be coated with roller pair 65 without adding any liquid additives or liquid substances. very large enough to cause permanent deformation of the monofilament cell walls in the panel. When pressure is applied, the fibers are somewhat crushed and the material thus treated is pulped without further treatment and used to produce armor paper and the like. used to.

Although the specific examples shown in the drawings have been described in connection with the treatment of cellulose fibers, this invention The method and apparatus can also be used to treat other natural fibers such as wool fibres. , and also man-made or It can also be used to treat artificial fibers.

From the above description, it can be seen that the method of the present invention does not require any use of liquid lubricants during high pressure processing. without crushing the fibrous material to produce smaller fiber sizes (higher SRo, e.g. SR’ 70-80), the fiber is impregnated during the high-pressure treatment. Adding a liquid substance to the reservoir, adding a lubricant at the same time, and possibly applying high pressure If additional liquid or solid substances are added after processing, e.g. fluffing or crushing When added immediately before or into the unit, typically -. and/or (hardware that gives abrasion effect) or in the case of solids that may clog the filter 44) The above materials are removed after the hammer mill or after the fibers are removed from the filter 44. Can be used for a wide range of processing of fibrous materials ranging from additive to It will be understood that it can be done.

´　Processing fibrous materials using high pressure processing without the use of substantial amounts of lubricants If the fineness of the fibers SR' is to be increased, the high-pressure treated material can be used as shown in Figure 3. In this case, a ``lubricant'' or ``coolant'' is added above. Appropriately added before the hammer mill or into the hammer mill as described above, or subjected to high pressure treatment. The treated material is taken out as it is after high-pressure treatment, then dried and crushed, or used for regular use. A wet pulping process is carried out. High-pressure processing is carried out in the presence of a liquid substance that penetrates the material. When used, the liquid substance usually acts as a "lubricant" and prevents fiber breakage. Stop.

According to a particular embodiment of the invention, a composite comprising, for example, hammer-type fibers may be used. Synthetic fibers are made of fibrous materials, and by crushing, organic bases (e.g. polymers) or inorganic bases ( prepared for incorporation into fiber-reinforced composites bonded by e.g. cement) It becomes a "fiber mixture." For example, 60% sulfate pulp, 30% Tocala fiber, "Composite paper" made of 6 pieces of 6-inch rayon fiber and 4% of 8mm rayon fiber. Can be crushed in a hammer mill. Obviously other fibers or materials mentioned above 1 composite paper” and some of these include sisal. ) fibers, coconut fibers, mineral fibers, and in some cases further reinforced fibers Polymer particles or particles constituting a base material or a part of the base material of a composite material that functions as a fiber Also includes fiber. Composite materials are created by incorporating the desired fibers in the desired ratio during papermaking. According to the embodiment of the present invention in which the fiber reinforced structure in the material is prepared, the resulting "composite paper" ” with or without impregnation with a desired impregnating agent and/or In combination, the above-mentioned high-pressure treatment is performed. In this way, Haton Processed fiber materials with strictly defined properties for a given purpose, without any limitation. can be manufactured.

According to a very important aspect of the invention, prior to high pressure treatment, in particular high pressure roller treatment, The liquid substance supplied to the dry fiber material is an impregnating agent, i.e. completely or partially. Agents that are introduced into fiber materials to impart desired properties to the fibers. Here, "impregnating agent" The term “bond” refers to chemically and/or physically bonded to fibers to form a substance between the fibers and the substance. means a substance that forms a permanent chemical and/or physical bond.

In this connection, the heating and heating of fibers, especially cellulose fibers, carried out according to the invention By compression and compression, the fibers are chemically activated to the desired extent, and the reaction added for this purpose is It will be understood that the property of reacting with sexual substances is strengthened.

The importance of heating fibrous materials is consistent with the above discussion and the present invention. One embodiment is to heat the cellulose-containing material to said temperature and after this the cellulose is formed by a method of reacting with a reactant capable of reacting with the hydroxyl group of the . Reactive substances, such as metal oxide acyl, after heating the material to the above temperature. Separation by metal oxide acyrate or isoananate The impregnation of ululose-containing materials is itself novel and can be used for various purposes, e.g. important per se for the manufacture of water-resistant liners (wrapping paper) and the like. It is.

One of the important impregnating agents that can be advantageously introduced into fibrous materials by the high pressure treatment of this invention is a so-called metal oxide acylate.

Metal oxide acylates include, for example, U.S. Pat. No. 3,087,949; No. 243,447, No. 3,177.238, No. 3,518,287, No. 3,518,287, No. No. 3, 625, 934, No. 3, "546, 262, No. 3,634" , 476 and 3.673,229, Belgian Patent No. 735, 548 , as well as British Patent Nos. 1,230,412, 1,274,718, and 1 ．． Organometallation described in No. 552,601 and No. 1,552,602 Contains compounds. The general composition of metal oxide acylate is Divalent metal: (R-Me-0-Me-R) X-ray compound, trivalent metal: (03- Me, -R3)y Planar compound, tetravalent metal: (06-Me4-R4) icosahedron It is expected to be a type compound. Here, Me is a metal atom, R is a carbon atom It is an acyl group which is an organic acid residue having a number of 12 or more, and X1Y and Z= 3-7 are the expected molecular sizes in solution. two or more different metals in each molecule, It is probably possible to make metal oxide acylates containing metals with different electric values. , and this type of compound also includes various other metal oxide acylates and mixtures thereof. as described in the above patent specifications. Metal oxide acylate and cell Its use in the impregnation of loin fibers was published June 12, 1980 with publication number WO8 International patent application A PCT/DK 791000 published as 0101176 Found in 55.

As is clear from the experiments described later, cellulose obtained by the high pressure impregnation method of this invention By introducing metal oxide acylate into the fiber, the content is very uniform over the entire cross section. fibers are obtained which have outstanding desirable properties for a variety of applications. Ru. Cellulose fibers are impregnated with metal oxide acylate by the method of this invention. If the metal oxide acylate is And it appears to bind to the fibers so that they cannot be removed. This “impregnated bond” ' is similar to the hydroxyl group in the chemical structure of metal oxide acylate and cellulose fiber. When cellulose fibers and polymerized metal oxides Based on a direct predominant physical bond with the sylate coating or a combination of these same effects. It will be based on

The metal oxide acylate impregnated cellulose fiber obtained by the method of this invention has a non-water absorbing property. is constantly decreasing and therefore remains dimensionally stable when placed in water or an aqueous slurry. It will be done. In this regard, for example, cellulose fibers impregnated with aluminum oxide acylate have been found to have substantially the same non-water absorption properties as, for example, polypropylene fibers.

Therefore, the present invention can be used in many applications requiring non-absorbent fibers having dimensional stability. Highly advantageous metal oxide acylate impregnated cellulose fibers are provided. .

According to certain embodiments of the invention, the fibers are coated with a coupling agent such as a silane and a metal acid. Processed in combination with compound acylate. Coupling agents and metal oxides The anlate can be added separately to the cellulose fibers or, as particularly preferred in this invention, According to a preferred embodiment, the coupling agent is a metal oxide acylate that is supplied to the fiber. Add both together by mixing. Surprisingly, as will be shown later by example As such, this combination improves the functionality of the metal oxide acylate or coupling agent. It has been found that no disadvantage arises due to this. Metal oxide acylate and sila The treatment of cellulose fibers in combination with coupling agents such as and this embodiment is limited to the method of introduction by high pressure treatment described above. (although high-pressure processing is currently the preferred method), e.g. effective containment, including introduction under high shear conditions, such as in a cell or the like. It is also within the scope of this invention to carry out the introduction by any suitable introduction method that can carry out immersion. It is within the range.

According to another highly advantageous embodiment of the invention, the metal oxide acylate and Preferably, the treatment of the cellulose fibers with a coupling agent further removes inorganic particulates. This is done in combination with applying it to fibers. As mentioned above, inorganic substances, for example, - Prior to processing in a fluffing unit such as a hair mill or a crushing unit. , or the granules can be applied to the fibers in a fiber mill, or the granules can be It can be applied to the fibers after they are removed from the lacrimal device 44. introduced Important examples of inorganic materials such as cement, silica, and silicon metabolites in electric furnaces include precipitated from the gas phase of the type obtained as a by-product of ferrosilicium production. In particular, ultrafine silica can be mentioned, and this ultrafine silica will be used in the example. I am using it. dimensionally stable fiber impregnated with metal oxide anlate with cement or silica; Cement bonding, for example in molded articles usually manufactured from asbestos-reinforced cement By applying it to the reinforcing fibers introduced into composite materials, cement-containing water-based The dispersion of fibers into the rally tends to be further improved. This with cement particles The amount of inventive cellulose fibers, cement and other additives that may be used Slurry for manufacturing fiber-reinforced cement-bonded materials by simply adding the exact amount of water be designed so that it can be prepared. Impregnated cellulose fibers, especially metal oxides Other types of particulate materials that are suitably incorporated into acylate-impregnated cellulose fibers include wood It is an adsorbent such as charcoal. Cellulose impregnated with metal oxide acylate supporting charcoal particles Ground fibers are the most useful type of absorbent, high-quality fibers for a variety of purposes. was found. In this case, too, the metal oxide acylate is Can be appropriately combined with pulling materials.

In addition, it is composed of cellulose fibers impregnated with metal oxide acylate supporting charcoal. This embodiment of the invention is limited to the specific high pressure method for producing fibers as described above. (although high-pressure methods are currently preferred), metal oxide acylates are other suitable methods used to impregnate and apply charcoal to the charcoal fibers. are also included within the scope of this invention.

Metal oxide acylate-hydrophobic cellulose fibers are mixed into an aqueous slurry, e.g. When introducing into a slurry, it is preferable to disperse it in water as easily as possible. Sparse The aqueous nature hinders to some extent the dispersion of the fibers into the aqueous medium. However, this invention According to certain embodiments, the dispersibility of such hydrophobic cellulose fibers imparts hydrophilicity. The introduction of one or more surfactants with the properties of It will be good. Surprisingly, cellulose fibers are impregnated with metal oxide acylates Although it is non-absorbent and therefore hydrophobic in nature, However, suitable surfactants or other types of interfaces that increase hydrophilicity or water dispersibility may be used. Hydrophilicity or dispersibility in aqueous media by introducing a combination of surfactants was found to be improved. As is clear from the experiments described later, this Nonionic or cationic surfactants are suitable for this purpose. even more surprising In addition, these surfactants do not need to be added separately from the metal oxide acylates. Of course, the surfactant can also be added separately, especially after the addition of the metal oxide acylate. ), together with metal oxide acylate, or mixed into metal oxide acylate. can be added. Another aspect of the present invention is metal oxide acylate The fiber is impregnated with a single or is composed of cellulose fibers containing multiple types of surfactants. As mentioned above, this According to an embodiment of the invention, the metal oxide acylate and/or surfactant described in this specification is Regardless of the method, it is not limited to cases where it is introduced by the high pressure impregnation method described above. Metal oxide acylates (or other useful hydrophobizing agents) and surfactants are introduced. Generally, such fibers are included in embodiments of this invention. However, the high pressure described in this specification Vacuum impregnation method produces hydrophobic cellulose fibers that disperse well in aqueous media This is the currently preferred method.

As is clear from the examples, metal oxide acylate impregnation and hydrophilic or aqueous medium one or more surfactants that modify the fibers in a way that increases their dispersibility. , introduction of a coupling agent, and application of inorganic particulates in a desired manner. It is within the scope of this invention to combine and also treat cellulose fibers. The above principles without the use of metal oxide acylates according to the specific end use of can also be combined.

As understood from the above description, the cellulose fiber of the embodiment of the present invention or its counterpart Cellulose fibers produced in accordance with aspects of the Act are designed for a wide range of purposes. , and useful. As reinforcing fibers for composite materials with inorganic or organic substrates The use of cellulose fibers according to the invention has already been described. Processed fiber of this invention Usage modes other than those mentioned above are as follows.

According to one aspect of the invention, the activated carbon treated metal oxide acylate impregnated fibers include: As adsorbed material, e.g. for liquid or gaseous adsorbed material, e.g. wine, beer. It is used for household chores, gas masks, etc.

According to a particular aspect of this application, the adsorbent furnace material loaded with charcoal or other adsorbent is hygienic. Used for supplies or napkins. Metal oxide anlate as desired Metals with antimicrobial activity as or as part of metal oxide acylate compounds Antibacterial effect on multi-fibers by using oxide acylates such as zinc oxide acylate can be given gender.

Cellulose fibers supported or bonded with activated carbon by applying activated carbon to cellulose fibers Obtaining fibers constitutes a particular aspect of this invention. According to this invention, activated carbon Not only metal oxide acylate treated cellulose but also impregnated or can be applied to any suitable cellulose fiber that is not impregnated, and This application can be carried out according to the method of the invention or by pulper or Application of activated carbon to cellulose fibers including application in hollander This can be done in any suitable manner for the application.

Cells treated with metal oxide acylate or impregnated with metal oxide acylate Advantageous alternatives to loin fibers, e.g. aluminum oxide acylate impregnated cellulose fibers The use of is used as an oil-absorbing furnace material, such as in the use of oil waste removal basins. Large amounts of To remove waste oil, the oil-absorbing cellulose fibers of this invention can be used in an unbound form. , in a bag designed to be attached to or removed from the area where the oil will be disposed of. pack.

Other uses of the fibers produced according to the method of the invention include, for example, dry laid With binding materials or binding fibers for reinforcing paper (dry 1aid paper), non-woven products, etc. It is used as a. For this purpose, binders, e.g. or has binding properties at temperatures below 150°C, for example from about 0°C to about 150°C. Properly impregnate the fibers with the polymer. Other uses of the impregnated fibers of this invention include , interlayer between hydrophilic layers in sanitary products and diapers or napkins, or their uses. It is used as a hydrophobic fiber, which is the outer layer of a product. For this purpose, hydrophobic metal oxide acylates or combinations of metal oxide acylates, e.g. The fibers are impregnated with aluminum stearate or talate.

Another field of use for the impregnated filters of this invention is their use as flame-resistant fibers. this For this purpose, conventional flame retardants or fire retardants, such as phosphorus- and/or chlorine-containing flame retardants, are used. and/or metal oxide acylates which are themselves flame retardant or fire retardant, e.g. The fibers are impregnated with antimony oxide acylate.

Other advantageous uses of the cellulose fiber impregnated with metal oxide acylate of the present invention are as follows: , for example as antistatic structures for glasses or lenses.

Details of the drugs used in the examples are as follows.

MOA C1460: Aluminum oxide stearate, white spirit medium 6 Solution containing 0% solids. Made in Switzerland, Lausacine, MOACOS, A.

MOAC 1400 Aluminum Dioxide Stearate, Solid.

Made by MOACO S, A, Lausanne, Switzerland.

MOA DF'-00,: Silicon-titanium alkoxide condensation oligomer, 1 00%. (An oligomer in which each silicon atom is bonded to a titanium atom via an oxygen bridge. be. Each silicon atom further has an epoxide group bonded to it. Each titanium atom has its own An impropoxide group is bonded on the primary valence. ) Flash point 30℃, metal content 1 Section 2.9 T1.3.8%Si, Switzerland, Lausanne, MOACO (MOACO) S, Made by A.

MOA DF-1400: Silicon-titanium alkoxide stearate (each silicon Atoms are bonded to titanium atoms via oxygen bridges. 3 epoxies on each silicon atom A do group is attached. Two stearyl groups are bonded to each titanium atom. ) pull A light brown waxy solid with a boiling point of 210°C and a metal content of 4.8% Ti and 5.6% Si. body. Made by MOACO S, A, Lausanne, Switzerland.

MOA DF-1000: Recon-tetratan alkoxytotalate. ), 1゛ space , Lausanne, made by MOACO (MOACO) S, A.

MOACDF-1400: Silicon-titanium-aluminum alkoxide steer rate. Made by MOACO S, A, Lausanne, Switzerland.

MOACOCC-1O-50-A: α-aminoethoxyaluminum-hydride Roxy Tallate. 50% solution in white spirinots. Switzerland, Lausanne, Mo. Made by MOACO S, A.

Manalox 4035olid: Formula where X is a stearate group (o= A solid polyoxyaluminum stearate represented by At-x). Al Minium content 8.8%. Viscosity ranges from 400P at 60℃ to 3 at 185℃ P o Manufactured by Manchem, Manchester, UK.

Manalox 205: Expressed by the formula (02At-X)m(At(OR)X2)n A polymerized organoaluminum compound having a composition as described above. This stuff has more saturated fat Contains about 25% solvent ester RX, which is the isopropyl ester of the acid. UK, Manufactured by Manchem, Manchester.

Manalox DPII/C/22P: Formula where X is a stearate group (0= A solid polyoxyaluminum stearate represented by AA-X)n. Al Minium content 8.6 inches. Viscosity range from 3.6P at 60℃ to 0.6P at 185℃. 25 P, freezing point below 90 degrees Celsius. Manufactured by Manchem, Manchester, UK.

BEROL 370: Ethylene oxide/furopylene oxide block polymer A nonionic surfactant consisting of: It has hydrophilicity (water solubility). This surface activity is This is the following circular.

The surface tension of Du Nouy is 25°C and 0.1% of active substance. 41 dyn/Cm.

Wet capacity of Draves, 7 g/l at 25°C, 25 seconds immersion .

Foaming of Rosu Miles (Ross-Miles), 50°C, 0. At 05% active substance, the immediate value is 5 mm.

0 friends after 5 minutes.

Sweden, Stenungsund Made by BEROL KEMI) AB.

BEROL 563: Alkyl-polyglycol ether ammonium methyl A cationic surfactant consisting of sulfate. It has the following surface activity.

The surface tension of Diunoy is 43 dyn/c at 25°C and 0.1% active substance. Wet capacity of IIL0 Draves, 10 g/l at 25°C and 25 seconds immersion .

Rossu Miles foaming, 50℃, 0.05% solution in hard water, 300ppm C In aCO3, the value immediately after was 100℃, and after 10 minutes it was 0.

Made by BEROL KEMIAB, Stenungsund, Sweden.

BEROL 572: Quaternary ammonium compound type cation field with antibacterial properties Surfactant. This surface activity is as follows.

The surface tension of Diunoy is 32 mN/m at 25°C and 0.1% active substance. .

Wet capacity of Drabes is 101/1 or more at 25°C and immersion time for 25 seconds.

Rossu Miles foaming, 50℃, 0.05% active substance, immediate value 1mm Om0 after 55 minutes BEROI, FINTEX 573: Alkyl polyglycol ether ammo A cationic surfactant and nonionic wetting agent consisting of Ni ethyl sulfate.

This surface activity is as follows.

The surface tension of Dininui is 35 mN/im at 25°C and 0.1% active substance. .

Wet capacity of Drabes, l/l/l at 25°C and immersion time 25 seconds.

Ross Miles foaming, 50℃, 0.05% active substance, immediate value 140 Me, 125 hours after 5 minutes.

Sweden, Stenungsund, BEROL KEMI AB Made.

5ilane A-175: r-methacryloxypropyl-tris (2-methacryloxypropyl-tris) A silane coupling agent consisting of (oxyethoxy)silane. Union Carnogui Made by Union Carbide 0 8ilane A-1100=consisting of 1-aminopropyltriethoxine run Silane cassilling agent. Union Carbide Made.

5ilane A-1102: T-aminolopyltriethoxysila/Karana Silane coupling agent. Union Carbide ) made.

5ilane A-1120: n-β-(aminoethyl)-γ-aminopropyl A silane cassilling agent consisting of rutrimethoxysilane. union carnoguido .

(Union Carbide) Q Silane Y-9566, 40%: Union Force - Manufactured by Noguid.

TES 40: Silicic acid ethyl ester having 91 to 9 silicon atoms per molecule. Wa Manufactured by Wacker Chemie.

Incyanate MDI Nidiphenylmethane-4,4'-diisocyanate.

Desmodur T2O and Desmodur T65: isomer 2,4-di Isocyanate toluene and 2,6-diisocyanate toluene in a ratio of 80:20 Ratio (DesmodurT80) and 65:35 ratio (Desmodur A mixture of two types containing T65). Made by Bayer.

MOBILWAX 2360: Melting point (ASTM D127) 75℃, needle penetration value (1/10 dragon) 26 at 25℃. 1501 at 42℃ flash point COC 276℃, 9 A microorganism with a viscosity (DIN 51562) of 11.4 cst at 8.9°C Ku + 7 tx.

ANTIBLAZE 78: Flame retardant, chlorinated phosphate ester, phosphoric acid content 12.0 %, chlorine content 34.0%, clear liquid that crystallizes at temperatures as low as 75°F.

VIRCOL 82: Chemically bonded, co-reactive flame retardant and Mobil Chemical Co., Ltd. Phosphorus-containing polyol flame retardant and flame retardant designed by.

Hydroxyl number (mti KOVg): 205 acid number (In9KOV&) : 0.3 Moisture content: None Functionality: 2 Phosphorus content: 11.3% Viscosity (cps at 23°C): 250 Ultrafine silica: Fine spherical SiO□ High dust content. Specific surface area (measured by BET method) approximately 250,000 (, nL2/ g, which corresponds to an average particle diameter of 0.1 μm. Density 2.229/CTL3゜ 5uper Rapid 4500: Ultra-fast Portland cement, specific surface area (black Raiy) 4500 CIrL2/fl.

Talc: Sedimentation analysis 10μmJ:Y) small, 93%, smaller than 5 μm, 81%; 2μmJ rainbow small, 35chi, Oil side (oil number) (DIN 53199): 56°MOBIL CERQ: Acid-stable microwax emulsion, solids content average 51%, wax coagulation Solid point: 65°C, particle size: 1-3 μm, manufactured by Mobil.

LUDOX) LS 40%: Silica particles made by DuPont Aqueous colloid dispersion. Stabilizing counterion: Sodium. Particle charge: negative. average Particle diameter: 12nmo Specific surface area: 230m/9゜AQUAPEL 3100 XL: Synthetic adhesive, protective coating that reacts with cellulose under neutral or alkaline conditions. 159% milk of alkyl ketin dimers with cationic starch derivatives as roids agent. Sweden, Cox 2019, Hizings 11/Gutsuka (l(isin) gsBacka), Hercules e Chemiska Actiberak (HerculQ) Made by s Kcmzska Aktiebelag).

KYMENE 557 H: Highly effective cationic active wet paper strength strengthening resin, po Reacrylamide shrimp chlorohydrin. Sweden, Box 2019, Hinn Nungus Backa, Hercules Chemise Power Actiberarch (Hercule) Made by Kemiska Aktiebelag).

MELMENT L 1020%: Concrete Superplasticizer: Salt ionic melamine 20% solution of resin.

CEM-MIX: Concrete superplasticizer: highly condensed naphthalene sulfone The sodium salt of the acid/formaldehyde condensate is typically Many consist of molecules containing seven or more naphthalene nuclei. Ten marks, a Made by Arlborg 1 Portland.

TRITON CF 10: Bennoer of octylphenyl polyethoxylate Stell.

AIRFLEX 120: Self-crosslinking vinyl-ethylene emulsion, Section 52, USA, PA, Wine (Wain e), Air Groducts Lu & Chemical GORI Co1o made by Air Products & Chemicals urleas: Fungicidal wood preservative oil. Tenmark, made by GORI.

5ilicone, curing: Wacke silicone rSilicone) Wacker 5t-DehAsiv Xl 00%, Addition-crosslinked resin IJ4 containing no solvent.

Cab-0-8i4: Colloidal silica particles, particle size approximately 1O~20μm0 Norit W 20: Activated carbon manufactured by Norit, iodine value 700/11 Apparent density 6009/l.

PVC solution: Composition: Pure PVC (without plasticizer) 50g 1 Tetrahydrofura 300g of methylene chloride, 500g of methylene chloride, and 0.5g of 5ilane A-1100. F.

Potassium water glass: Be'28~30° exposed sulfuric acid pal f: sheet weight approx. 750 ．． ! 9//rr+2°Sweden, StoraKopp Manufactured by arberg).

CTMP parno: chemical-thermal mechanical pulp. A bleached sulfuric acid cell with an SR' of about 16 It consists of about 85% thermo-mechanical pulp having about 15% ululose and an SR' of about 16.

The pulp is free of anti-binding agents and other agents. Seat weight approximately 750g/m.

Straw Cellulose: Sulfite pulp made from rye and wheat straw. SR’ approx. 32° Ten Mark, Frederinia Cellulosefabrik (Fredericia Ce1lulosefabrik).

In the following examples, the treatment agents or combinations of treatment agents described are It was fed to the cellulose web IO through the cellulose web IO as long as it did not break. In other words, the heating unit 27 and the heating jacket of the supply conduit 26! 11,200℃ (other temperatures listed) (if not already present) and the amount mentioned in the example, while passing through the tunnel 20, approx. It was added to 10 kg of dry, bleached sulfate cellulose heated to 110°C. some examples Add additional material to the hammer mill 19 at or before the hammer mill 19. Ta.

Processing agent addition amount g/lokg Example number 1234567 MoA C146010001000100100OC1400600 ■ACOCC-1O-50-A 600M0A D 1200 600 Manalox 4035olid 600M0A D-0060 M0A DF-0060 Example number 8 9101112131415M0A C146010001000 10001000100010001000Man100O403Sol id 600M0A DF-140060 M0A DF-100060 M0A CDF-140060 BEROL370 3030151515BEROL 563 151515 Silane A-1100303030Silane A-110230 ~ MOA C14605005005001000100010001000MO BI100O2360300 ANTIBLAZE 78 300 vIRcOL 82 300 1ROL370 15 15 15 15BEROL563 15 15 15 Addition to 15Silane A-110030303030 hammer mill Ultrafine silica 5000 1000 Super Rapid 4500 4000 Smoked silicon ± 5000 Plaster 5000 Example number 2324252627 2829 30M0A C14601(X)t ) 1000100010001(X)010001011) 1(X)OBE ROL 370 15 15 30 6f) BEROL 563 15 15 Addition to Silane A-11003030303030 Hammer Mill ・Boyaki silicon clay crime sword Talc J■) Wolastonite seal (1) Iron powder painting Example number 31 32 33 '34 35 36 37M0BILCERQ' 500 500 1000 1000 500 500LUDOX H840 %500 Potassium water glass 500 Boric acid 30% 250 ALMID 750% 500 Ammonium sulfate 30% 100 AQUAPEL 3100 XL 1000Silane A-110050 S i l ane Y-956640% 50M0BILCIJ Q 500 500 round pieces Pan-LUDOX H340% 400 Potassium water glass 400 5tX) Boric acid section 30 ALMID 7 50% AQUAPEL 3100 XL 500 500450450250KYME NE 557 H50 MFJ Hiriso L102 staff 1 (1) Lecture C-MIX50 St 1ane Y-956640% Gloss TRITON CF 10 50 GORI Co1ourless*1 (XX) Silicone, curin g* 1(XX) pvc solution* phlegm MDA　C14601αηlαη1αηlα Spraying into the car oven mill 5ilane A-11001CO30021JJMOA I)-005002 [X) Potassium water glass 1 (XX) Cab -0-8i 1 500 Ethanol 1500 H mark for 2-nolopanol l Methylene chloride general *Added at room temperature MOA C146037 2m1 (X code DI (1-port)--1Of) port) C/' Marmil medium/spray 5ilane A-IH f’3006060601 (ItMOA D-0060 60120 Cab-0-8i l 1■ Ultra-fine powdered fish Ethanol** 1500150015 (η1 Shiba Takumi α■6 sword 1shiη2-Propa Tool 1000 BEROL 370 15 BEROL 563 15 BEROI, 572 30 * Added at room temperature ** MOA added even before high pressure roller C1400500500500 M0A DF-1400500500500400400M0A DF-002 00200400TES 40 200 200 TES 40+ 5ilane A1102 Ratio 96:4 200 200 400M0A DF-1400400 M0A DF-00200 TES 40 400 300 M0A C1400500500 Manalox 4035 solid 500 500 Manalox 205 500 TES40 150 150' 150Silane A-1753030 BEROL 370 15 15 Example number 78 79 80 81 82 82 83 84 -Manalox 205 500 600Silane A-17530 BEROL 370 15 D.I. Desmodur T2O500 LUDOX H840% 200 Potassium water glass 300 TES 40 too 100 Example number 85 86 87 88 89 90 91 92M0A c1400 500 500 500M0A DF’-1400500500500400 400M0A DF-00200200400TES40 - 200 200 TES 40+ 5ilane A1102 Ratio g6; 4 200 200 400 Example number 93 94 95 M0A DF-1400400 M0A DF-00200 TES 40 400 300 Dry the sulfate cellulose pulp and do not add any liquid before rolling. The sample was passed through the rollers at a maximum pressure C of about 10,000 kp) without any pressure applied.

The rolled product has a tobacco flake-like appearance and is considerably smaller than the starting fiber. It is thought that it has been miniaturized. When dispersed in water, the fibers precipitate and their density decreases. showed that it was high. Paper made from this fiber in a laboratory sheet-forming machine is produced using sulfuric acid. The fibers were paper-like and showed a fairly high SRo. This paper has high tensile strength Although it is strong, it has low tear strength like parchment paper.

A liner (wrapping paper) made from sulfate cellulose is dried at 200°C. child The metal oxide anhydride is then added, preferably undiluted and heated to about 200°C. rate (aluminum oxide tallate or stearate, or zinc oxide tally) (or stearate). The impregnated paper thus obtained is used as such. or preferably subjected to a roller treatment as previously described. profit The impregnated liner is made of ivy that is waterproof (water resistant). Metal oxide acylate oxidizes When zinc acylate, the liner is further resistant to fungi. similarly for example, treating sulfate pulp and high-pressure roller treatment or roller treatment. – Can be used as is without treatment, in which case it can be used, for example, on the back of carpets. roofing paper or cement materials as well as phenolic resins and polyesters. The device shown in Figure 3 can be used as a sheet-type reinforcement for plastic materials. In, about 700,! i'/m2 sheet weight and does not contain any drug Unbleached sulfate 7-pulp (flujj pulp) to 500 kFl , 70% aluminum oxide stearate solution in 100# white spirit. Impregnated. The impregnating material is 3.5 to 9 5ilane A-1100 and 3.5 #BEROL 370'! mixed with. Mix this mixture in advance to approx. 90 to 1 Heated to 00°C. The fiber web is heated to a temperature of approximately 140°C just before impregnation. It was hot. This fiber was used to create Eterna in the Perufloon Eternite aircraft. An Eternite type cement material was manufactured. Treated fiber 14 Slurry the fibers by pulping for 20 minutes in 50,000 to 90% water. did. The slurry thus obtained has a capacity of 3 tons, calculated on the basis of the cement introduced. Cement slurry and ultra-fine glue force of about 50 IC9 were fully applied. Fiber dispersion and Both were easy to introduce into cement slurry. In the log of the machine, Strong cationic polymer electrolysis of approximately 1% based on the dry content of the slurry is applied to the fiber slurry. Quality (Sueten, Box 2019, Hinongsbacka, Hercules Chemiriki Actibolag) was added just before dehydration. Retention was excellent. panel It was cured according to a conventional method. This one has a dimensional stability of about 32 SR”!f. Tomato-shaped straw cellulose lO! j, activated carbon with a specific surface area of 700 m2/if2. 5.9, and 2.5 g of activated carbon having a specific surface area of 1400 m2/& of 1000- Suspended in water, the slurry is then dehydrated and synthesized in a laboratory note-forming machine. It was dried into a sheet.

Activated carbon retention was outstanding. There is virtually no charcoal in pack water and it is incorporated into fibers. It took hold.

Description of the fibers produced in the examples.

Examples 1-5: The fibers had good hydrophobicity.Example 6-1O1 bifibers were cement laminated. It was suitable for introduction as a reinforcing material for the base material.

Examples 11-15: The fibers do not absorb water and are soluble in e.g. cement-containing slurries. It showed excellent properties in terms of easy dispersion.

Example 16: This fiber is somewhat more durable than a fiber impregnated with metal oxide anlate only. It was fragile. These include, for example, polymers such as polyurethane or polyester. It is expected that it will be useful as a reinforcing material.

Examples 17 and 18: In this example, the fibers were impregnated with a fire retardant. chloroparaf A similar experiment was conducted using fin.

Examples 19-24: In these examples, the fibers are coated with metal oxide acylates and surfactants. impregnated with a combination of agents, which do not absorb water and therefore do not swell; However, the introduction of surfactants makes it sufficiently hydrophilic and easily dispersed in aqueous slurries. A stabilized fiber was obtained. Furthermore, these fibers are was reversed by adding particulate material.

Examples 25-27: The fibers produced in these examples are It exhibits excellent adsorption properties and can be used, for example, as a filter material for liquids or gases, e.g. Gas can be used as a material for pouring alcohol or beer, as a furnace material for household use or in the kitchen. It is useful as a p-material for masks and as a reactor material for drinking water.

Examples 28 and 29: The fibers produced according to this example can be used especially for cement, gypsum, etc. Useful as reinforcing fibers.

Example 30: This fiber is useful as a hydrophilic media fiber for soilless plant cultivation. It is also useful as a furnace material.

Examples 31-36: These experiments also apply to Method A of this invention: aqueous dispersions, solutions, etc. This was done to show that it can be used. Even when impregnating water-based materials, Sufficient drying with Channel 20 ensures rapid penetration, This drying process is very advantageous.

Example 38: In this experiment, the applied latex was was removed and remained on the web. This is undesirable. Higher film formation It is preferred to use a dispersion having a temperature higher than 110°C, for example. Dew.

Example 39: The fibers obtained in this example showed excellent hydrophobicity and fire retardant properties.

Example 40: This fiber was relatively brittle and hydrophobic, and had no fire retardant properties.

Examples 43 and 45: The fibers had excellent dispersibility.

Examples 46 and 47: The fibers exhibited good overall hydrophobicity.

Example 48: This fiber is useful as a filler for pillows, as an insulating material for fabrics, etc. is expected. This fiber is very smooth and easily slides over each other.

Example 49: This fiber is suitable as a binding fiber in non-woven structures, for example dry paper.

Examples 50-56: In these experiments, metal oxide anlates were combined with other agents. ・Can be combined with other drugs by adding it during the hammer mill or just before the hammer mill. Used together. Although excellent fibers were obtained, other methods such as those shown in Examples 11-15 Preferably, the agent is added to the metal oxide acylate.

Example 57: This fiber had very special properties. This fiber is brittle and has no plasticity. and when used in papermaking, it is difficult to compete with each other, rather it is very fluffy. It became a structure.

Example 58: In contrast to Example 57, the fibers produced in this example They retained their mutual bonding properties even after being combined, filtered, and dried.

Examples 62-72: These fibers are introduced into the quantification panel at (4-10 weight factors) very suitable for

Examples 85-95: Straw cellulose, the fibers are very small, so following these examples The impregnated fibers produced by Very suitable as a moisturizing agent.

Fibers produced according to Examples 1.11, 12.13.19 and 20 above, respectively. The following tests were conducted regarding:

The fibers produced according to Example 1 were heated in dichloromethane and in a Soxhlet apparatus, respectively. and extracted using petroleum ether. 5.2 of substances applied by dichloromethane % was extracted and 4.5% of the substance applied to petroleum ether was extracted. . This is approximately half the weight of the applied aluminum oxide stearate.

Elemental analysis of aluminum oxide stearate is C: 66.3, H: 10.7 , o: 14.7, ht: 8.3, but the two extracts are Elementary analysis showed the following composition.

Petroleum ether extract C: 77.5, H: 13.1.

0: 9.1=99.7 Dichloromethane extract C: 77.7, H: 13.5, o: 9.2 = 100.4 This result indicates that the extract does not contain unreacted aluminum oxide stearate. Given that there is no aluminum present, perhaps the extraction The substance must be stearic acid that was present in excess in aluminum oxide stearate. cormorant.

Figure 7 is a scanning electron micrograph showing the distribution of aluminum in the treated web. (SEM) (magnification x 54). It was noted that the distribution was very flat. Good morning.

Figure 8 is a fiber + 7) SEM (magnification XI 10), and some fibers are non-fibers. It is always crushed, indicating that other fibers are round.

This also applies to Figures 9 and 10, which show single fibers extracted with dichloromethane (magnification It is also clear from x930 and x1570, respectively.

Figures 11 and 12 (magnifications are X2050 and X3000, respectively; Dichloromethane-extracted hawk fibers (Figure 11) and intact fibers (Figure 12), respectively. Brazing, fiber ends (Fig. 11) and fiber surfaces (Fig. 12) are different from normal pulp fibers. It shows that it always has a different appearance.

Contact angle and absorption measurements of fibers (extracted and unextracted) The test consisting of shows that the surface of the fiber is clearly hydrophobic and lipophilic. Ru. It has also been clearly found that the fibers do not swell in solvents. Furthermore, the fiber It is clear that it retains its hydrophobicity even after extraction.

The water retention value (WHV) of the fibers was measured. The results are shown in the table below. This table also includes The content, contact angle, and wetting properties of the fibers are indicative.

Example 1 93.9 44.4110 -25 Example 19 93.2 39.5 88 2.5 Example 11 92.5 55.1 86 5.1 Example 13 93.7 63.2 89 1.3 cases 12 93.2 50.0 83 8.9 cases 20 93.0 43.2 92 0.0 Polypropylene fiber 49.0 Polyethylene fiber 98.3 16.4 exposed sulfate Pulp ~94 172 *Wettability = γ x animals φ A thermal analysis of the fiber produced according to Example 1 revealed that the endothermic reaction occurred at 50°C. It was shown that the reaction started at 5120°C and was completed at 85°C. reaction corresponds to approximately 5% water removal.

An exothermic reaction occurs between 275°C and 335°C. This is due to thermal decomposition. weight reduction is 66%. After this, an exothermic reaction occurs again at 400-450°C. child This corresponds to ignition and combustion of the remaining material.

The above results indicate that the fiber is thermally stable up to 275°C and that the zeta potential is This shows that it corresponds to the zeta potential of normal pulp.

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Claims (1)

[Claims] ■ fibers each having a portion or external surface portion constituting interstices or pores; heat treatment and/or drying treatment to the material containing the material, and then fill the gaps or air the fibers are natural fibers, e.g. Cellulose fibrils containing naturally occurring cellulose fibrils, such as sulfate pulp and sulfate pulp pulp, TMP and CTMP pulp, hardwood pulp and softwood pulp, straw cellulose Cereals containing pulp, cellulose pulp, wood chips, sawdust, cotton, or synthetic or is regenerated cellulose, saijun, or wool, ・Toshiyoshi, kapok, sisal, red 7a, The method according to claim 1, wherein the fiber is coconut fiber, or cotton. , 3. Material The material is pressurized to a degree sufficient to permanently deform the membranes of at least some of the fibers. The method according to claim 1 or claim 2. 4. Claims 1 to 3, wherein the material is a fibrous sheet or web material. The method according to any one of the above. 5. A claim in which the compression is performed by applying roller treatment to the material. The method according to any one of the items 1 to 4. 6. A claim for applying a liquid substance to said material prior to or during said compaction. The method according to any one of Items 1 to J5 in the range 1. 7. Claims for applying liquid substances to materials following heat treatment and/or drying treatment The method according to any one of the ranges 1 to 6. 8. Pass through the roller gap formed by the pair of rollers that continuously grind the material. Any one of claims 1 to 7, wherein the roller treatment is performed by tightening. The method described in Section 1. 9. Adding the liquid substance and/or additional liquid or particulate additive to two adjacent 9. The method of claim 8, wherein the method is applied to said material in the middle of a pair of rollers. lO1 The liquid substance is preferably applied to the material by an airless atomization technique. 4L4. The method according to any one of claims 6 to 9. 11. The liquid substance is applied to the material through a nozzle that supplies the liquid in a pulsating manner! li j. The method according to claim 1O, which comprises misting. 12. Claim in which said liquid substance is applied to said material from at least one roller. The method according to item 9. 13. Applying said liquid substance with material G from a roller immersed in a container of said liquid substance. The method according to claim @12. 14＠The liquid substance λ is discharged from a roller to which the liquid substance is discharged and fed at a rapid rate. 13. A method according to claim 12, wherein the method is applied to a material. 15. At least one of the rollers used in the roller treatment is heated. The method according to any one of the ranges 1 to 11. 16 After compaction, the material is crushed in a mill or other fluffing device. The method according to any one of claims 1 to 15. 17. During or prior to crushing in a fluffing device after said compression, 17. The method of claim 16, wherein a lubricant is added to the material. 18. Applying activated carbon to the material prior to and/or after compaction. The method according to any one of claims 1 to 17. 19. Adding activated carbon while crushing the material in a fluffing device such as a hammer mill. 19. The method according to claim 18. 20. Any one of claims 6 to 19, wherein the ti-like substance is an impregnating agent. The method described in section. 21, the impregnating agent is one or more metal oxide anlates, such as aluminum oxide Mustearate or tallate, or approximately 50% aluminum oxide stearate Tomoshikunmatarate and about 50 inches of alkali/-titanium alkoxide/decondensed orico Claim 20, which is a combination with 22. Roll means comprising at least one pair of rollers, the pair of rollers having grooves formed therein; a supply means for supplying all of the fibrous material to the nip between the rollers to be supplied; including heating and/or drying means for heating and/or drying the fibrous material; For carrying out the method according to any one of claims 1 to 21, Device. 23. for applying a liquid substance to the fibrous material upstream of the rolling means; 23. The apparatus of claim 22, further comprising means of. 24. The liquid substance applying means supplies a nozzle and a pulsating flow of the liquid substance to the nozzle. 24. The apparatus of claim 23, comprising means for: 256 The fibrous material is completely heated and/or dried upstream of the liquid substance application means. The device according to any one of clauses 22 to 24, further comprising means for Place. 26. Further comprising means for crushing the fibrous material downstream of the roll means. 26. A device according to any one of claims 22 to 25. 27. The crushing means includes a hammer mill (equipment described in required range item 26) Place. 28 Comprising natural fibers with air/ground walls permanently deformed by compression 4 , quality material. 29. The fibrous material according to claim 28, comprising cellulose fibers. 30, impregnated with metal oxide anlate and/or supported with activated carbon particles The fibrous material according to Range 29. Impregnated with 31° metal oxide anlate and coupled with a coupling agent such as 7Ran. Contains cellulose. 32 Metal oxide anlate'f-impregnation and dispersibility of fibers in aqueous media Cellulose 1 Weifu contains one or more surfactants to increase the 33 Manufactured by the method according to any one of claims 1 to 21 Cellulose according to any one of Items 29 to 32. 34.1 Treatment of fibers with metal oxide anlate containing coupling material A method for impregnating cellulose-1 fibers comprising: 35. The method according to claim 34, wherein the force and the pulling agent are Nran. 36. The method according to claim 34 or 35, wherein the treatment is carried out under high shear conditions. . 37, the method according to any one of claims 6 to 21, and gold and pyrolic acid. Combining the compound anlate and the coupling agent that constitutes the liquid layer 4'. A method according to claim 34 or 35. 38 Metal oxide anoleate and particulate matter 4. consists of applying to usu Cellulose 1. How to process sashimi. 39 It is possible that the particulate matter is ultrafine phosphoric acid and/or cement precipitated from the gas phase. The method according to claim 3-8. In case of 40.7Kk loss, steel fiber will be used to manufacture 11R reinforced cement bonding material. The method according to claim 39, in which the amount of cement lathe is added to form a slurry. . 41. The method of claim 38, wherein the particulate material is an adsorbent coarse material. 42. The method of claim 41, wherein the adsorbent particulate material is charcoal. 43, carried out by the method according to any one of claims 6 to 21. 43. A method according to any one of claims 38 to 42. 44, impregnated with metal oxide anlate, and further improved the properties of the fiber with a large parent material. Cellulose containing one or more surfactants to modify it to be aqueous a Usui. 4↓5 Impregnation of metal/metal acid ratio anlate and impregnation of surfactant that imparts affinity to parent/metal acid anlate Cellulose impregnated with metal oxides, especially for introduction into aqueous slurries, consisting of A method for manufacturing fibers. 46. Claim 4, wherein the surfactant is a nonionic or cationic surfactant. The method described in Section 5. 47. By mixing surfactants into metal oxide acylates in some cases, 47. The method of claim 46, wherein the metal oxide is added together with the metal oxide. 48, metal oxide acylate and/or surfactant in claims 6 to 2 Claims 45 to 47 introduced by the method according to any one of paragraph 1. The method according to any one of the above. 49° Coupling agent and/or particulate material further added to the fibers Claim 4 The method according to any one of Items 5 to 48. 50. Adsorbent fibers comprising activated carbon treated metal oxide impregnated fibers. 51. Sanitary products or nanokins comprising the fiber according to claim 50. (diaper). 52. Claim 51 that the metal oxide acylate or a part thereof has antibacterial properties Sanitary products or nanokins (diapers) as described in section. 53. Claims in which the metal oxide acylate or a part thereof is zinc oxide acylate Sanitary products or napkins (diapers) as described in Scope 50. 54. Oil-absorbing fiber comprising cellulose fiber impregnated with metal oxide acylate. 55. Claim No. 55, wherein the metal oxide acylate is aluminum oxide acylate. The oil-absorbing fiber according to item 54. 56 Claim 54 or 55 packed in a permeable bag in an unbound form The oil-absorbing 1 fiber described in . 57. Metal oxide acyl as an intermediate layer between hydrophilic fibers and as an outer layer of the product Sanitary materials and diapers or napkins comprising impregnated hydrophobic cellulose fibers. 58, the metal oxide anlate is aluminum oxide stearate or tallate A sanitary article according to claim 57. 59. Antistatic tissue comprising cellulose fibers impregnated with metal oxide acylate. 60, cellulose fiber impregnated with incyanato. 61, produced by the method described in any one of claims 1 to 21. Cellulose fiber according to claim 61. 62. Claims in which the impregnating agent is present in 4 to io% by weight, in particular 6 to 8% by weight on dry matter Any of Items 30 to 33, 44, or 60 is the impregnated cell according to Item 1. Loin fiber. 63, any one of claims 30 to 33, 44, or 60 A composite material comprising the mentioned fibers. 64, applying pressure to a degree sufficient to permanently deform at least some of the cell walls of the fibers. A composite material containing compressed fibers. 65, materials containing natural or synthetic cellulose fibers at 100-275°C, especially 120°C -250°C, preferably about 160-220°C, more preferably 180-200°C natural or natural materials consisting of heating to a temperature of is a method of impregnating synthetic cellulose fibers. 66. Claims in which the impregnating agent comprises metal oxide acylate or incyanate i The method according to paragraph 65. 67. The method of claim 65 or 66, wherein the material is compressed after heating. 68, for claims where the material is pulp, or wet or dry sheets or webs. The method according to any one of the ranges 65 to 67. 69- Claims that the impregnating agent is a drug that reacts with the hydroxyl group of carulose The method according to any one of paragraphs 65 to 68.