JP6137525B2 - Method for producing amorphous cellulose - Google Patents

Description

  The present invention relates to a method for producing amorphized cellulose.

  In recent years, from the viewpoint of depletion of fossil fuels and environmental problems, interest in woody biomass resources, which are renewable organic resources, has increased.

  However, when considered as an industrial material, cellulose, which is a main component of woody biomass, has a very complex and strong crystal structure, and therefore has poor applicability. Therefore, when used for bioethanol or the like, it must be amorphized in advance.

  Amorphous materials obtained from these woody biomass resources are expected to have a wide range of applications from the industrial field to the food field in addition to bioethanol.

  However, the existing amorphous technology has many problems such as high cost and low productivity. Therefore, development of a technique that can be easily and efficiently amorphized in a short time is currently required.

  As conventional techniques related to efficient amorphization, Patent Documents 1 and 2 propose a technique for amorphizing a cellulose-containing raw material using a medium pulverizer or the like.

  Moreover, although the present inventors are not a cellulose containing raw material, they succeeded in making amorphous rice starch in a short time by adding heat and shear simultaneously and grinding (Patent Documents 3, 4, and 5). .

Japanese Patent No. 4160108 Japanese Patent No. 4160109 Japanese Patent No. 4767128 JP 2009-213472 A JP 2010-215861 A

  However, as described above, there are few technologies that can satisfy the cost, productivity, and efficiency when reducing the crystallinity of cellulose, and there is a need for a new technology that can efficiently and easily amorphousize cellulose in a short time. Yes.

  The present invention has been made in view of the circumstances as described above, and it is an object of the present invention to provide a method for producing amorphous cellulose that can easily and efficiently amorphousize a cellulose-containing raw material in a short time. It is said.

  In order to solve the above-mentioned problems, the method for producing an amorphous cellulose of the present invention comprises a step of pulverizing a cellulose-containing raw material by applying a shearing force under a temperature condition of -5 to 40 ° C. to make the cellulose amorphous. It is characterized by including.

  In this method for producing amorphous cellulose, it is preferable to pulverize the cellulose-containing raw material by applying a shearing force under a temperature condition of -5 to 25 ° C. to make the cellulose amorphous.

  In this method for producing amorphous cellulose, the cellulose-containing raw material is preferably a piece of wood.

  In this method for producing amorphous cellulose, it is preferable to apply a shearing force to a cellulose-containing raw material having a water content of 0.5 to 20% by mass to grind it.

  In this method for producing amorphous cellulose, it is preferable that the gap between two relatively moving members is 0.5 mm or less and a cellulose-containing raw material is introduced into the gap to give a shearing force and pulverize.

  According to the present invention, a cellulose-containing raw material can be amorphized simply and efficiently in a short time.

BRIEF DESCRIPTION OF THE DRAWINGS It is the schematic (top is a top view, the bottom is a side view) which shows an example of the apparatus structure for enforcing the method of this invention. It is principal part sectional drawing of the apparatus of FIG. It is a wide-angle X-ray diffraction graph of the powder obtained by using hinoki as a raw material and changing the temperature conditions and crushing. It is a graph which shows the relationship between a grinding | pulverization temperature and the particle size distribution of the hinoki after pulverization. It is a wide-angle X-ray diffraction graph of the powder obtained by using hinoki as a raw material and changing the water content and crushing. (A) shows a result with a water content of about 1% by weight, and (b) shows a result with a water content of about 20% by weight. It is a wide-angle X-ray diffraction graph of the powder obtained by using hinoki as a raw material and changing the rotational speed of the mortar and grinding (heat removal (15 ° C.) and heating (140 ° C.)). (A) shows the result of heat removal pulverization (15 ° C.), and (b) shows the result of heat pulverization (140 ° C.). It is the wide-angle X-ray diffraction graph of the powder obtained by changing the temperature conditions using the Japanese cypress infiltrated with ethanol as a raw material. It is a wide-angle X-ray diffraction graph of the powder obtained by using high-purity crystalline cellulose fiber (commercially available product) as a raw material and changing the temperature conditions and pulverizing. It is a graph which shows the relationship between a grinding | pulverization temperature and the cellulose crystallinity of a grinding | pulverization processed material. It is a graph which shows the measurement result of the particle size distribution of the cellulose simple substance after grinding | pulverization according to grinding | pulverization temperature. It is the graph (left) and photograph (right) which show the relationship between a grinding | pulverization temperature and the particle size distribution of the cellulose simple substance after a grinding | pulverization. It is a wide-angle X-ray diffraction graph of the powder obtained by using high-purity crystalline cellulose fiber (commercially available product) as a raw material and changing the temperature conditions and pulverizing. FIG. 5 is a graph in which saccharification characteristics under untreated, 15 ° C. pulverization, and 140 ° C. pulverization conditions in the case of using cedar wood chips as a raw material are arranged with glucose concentration on the vertical axis and time on the horizontal axis. 6 is a graph in which saccharification characteristics under untreated, 15 ° C. pulverization, and 140 ° C. pulverization conditions in the case of using beech wood pieces as a raw material are arranged with glucose concentration on the vertical axis and time on the horizontal axis.

  The present invention is described in detail below.

  The inventors of the present invention studied the amorphization (alphalation) of a cellulose-containing raw material based on the techniques of Patent Documents 3, 4, and 5 for making rice starch amorphous. However, the cellulose did not become amorphous at all under the heating conditions for making the rice starch amorphous as in Patent Documents 3 and 4. However, the present inventors have found that the amorphousization of cellulose occurs specifically within a specific temperature range of the heat removal condition, and completed the present invention.

  Specifically, the cellulose-containing raw material is -5 to 40 ° C (lower limit is preferably 0 ° C or higher), preferably -5 to 35 ° C (lower limit is preferably 0 ° C or higher), more preferably -5 to 30 ° C ( The lower limit is preferably 0 ° C or higher), more preferably -5 to 25 ° C (lower limit is preferably 0 ° C or higher), particularly preferably -5 to 20 ° C (lower limit is preferably 0 ° C or higher), most preferably -5. Cellulose can be made amorphous (alpha-ized) by applying shearing force under a temperature condition of ˜15 ° C. (lower limit is preferably 0 ° C. or more) (Examples after FIG. 3 and particularly FIG. 12). Etc.).

  In the present invention, the cellulose-containing raw material can be used for woody materials such as cypress, cedar, beech and bamboo, and so-called soft cellulose such as paper and grass.

  Moreover, as a cellulose containing raw material, a cellulose simple substance, for example, commercially available crystalline cellulose, can also be used. The cellulose I type crystallinity (see Examples) of commercially available crystalline cellulose is usually 80% or more.

  The cellulose I-type crystallinity of the cellulose-containing raw material used in the present invention is preferably 50% or more, and more preferably 70% or more. According to the present invention, the crystallinity of the cellulose-containing raw material having such high crystallinity can be greatly reduced.

  The form of these cellulose-containing raw materials is not particularly limited, and various forms such as chips, fibers, granules, and powders can be used. When using a wood piece as the cellulose-containing raw material, the size is preferably 2 to 5 mm square in the case of a chip-like material, for example. Thereby, grinding can be performed efficiently and easily.

  In the cellulose-containing raw material used in the present invention, the cellulose content (total amount of cellulose and hemicellulose) in the remaining components excluding water is preferably 20% by mass or more, more preferably 40% by mass or more. When a material in such a range is used, an amorphous cellulose roll can be produced efficiently.

  The water content in the cellulose-containing raw material is preferably 0.5 to 20% by mass. If the water content in the cellulose-containing raw material is within this range, it can be easily pulverized and the crystallinity of cellulose can be easily reduced by pulverization.

  In addition, there is no limitation in particular as a method of removing water from a raw material, For example, vacuum drying, drying by dry air, etc. are applicable.

  FIG. 1 is a schematic diagram showing an example of a device configuration for carrying out the method of the present invention.

  The apparatus 10 includes an upper mill 11 that is fixedly installed, and a lower mill 12 that is rotatably provided between the upper mill 11 via a predetermined gap 13.

  The upper mill 11 is formed in a ring shape having a raw material inlet 14 for introducing a cellulose-containing raw material in the center. The insertion port 14 communicates with the gap 13 on the bottom surface of the upper mill 11. The lower mill 12 is formed in a disk shape having substantially the same outer diameter as the upper mill 11.

  The lower mill 12 is rotationally driven by a motor 15 at a predetermined speed. The gap 13 between the upper mill 11 and the lower mill 12 can be adjusted within the range of the gap adjusting section 16, depending on the cellulose-containing raw material used as a raw material, the size of a desired powder to be obtained after processing, and the like. Preferably it is 0.5 mm or less, More preferably, it is 0.1 mm or less, More preferably, it can be in the range of 0.005-0.05 mm.

  In the upper mill 11, an antifreeze liquid is circulated from the thermostatic bath 29, and the cooling temperature is controlled by the antifreeze liquid.

  The upper mill 11 is provided with a heater 17. The heater 17 is formed in a ring shape having substantially the same outer diameter as the upper mill 11 and an opening having substantially the same diameter as the raw material inlet 14. The heater 17 is connected to a temperature controller 19 through a heater cord 18 and heats the upper die 11 by heating to a temperature set by the temperature controller 19. Furthermore, when cooling, the temperature of the mortar at the time of pulverization can be controlled by circulating water or antifreeze liquid whose temperature is controlled by a thermostat in the mortar. In addition, in order to control the temperature of the mortar part with higher accuracy, a Peltier type Peltier element 17 having substantially the same shape (ring shape) is installed instead of the heater 17 provided on the upper mortar 11. A temperature control device can be configured, and this enables high-precision temperature control from, for example, -20 ° C to 120 ° C.

  The computer 22 compares the set temperature by the temperature controller 19 (input from the data cable 23) with the measured temperature by the thermocouple (not shown) (input from the data cable 21), and the heater via the temperature control cable 24. A control signal is supplied to the temperature controller 19.

  Further, the computer 22 gives a motor control signal to the motor 15 via the motor control cable 25 to control the number of rotations of the lower mill 12 by the motor 15.

  The rotation speed of the lower mill 12 is preferably 80 to 380 rpm, more preferably 80 to 180 rpm. If it is in such a range, the shear rate which the cellulose containing raw material thrown into the gap 13 receives between the fixed upper die 11 and the rotating lower die 12 can be made appropriate.

  A tray 26 having an inner diameter sufficiently larger than these outer diameters is provided below the upper mill 11 / lower mill 12. A dropping port 27 is opened on the bottom surface of the tray 26. The amorphous cellulose after the processing by the apparatus 10 is dropped from the tray 26, and further stored in a predetermined container (not shown) through a dropping chute 28. I try to let them.

  As shown in FIG. 2, which is a cross-sectional view of the main part of the apparatus 10, the upper mill 11 has a raw material passage 11c from the inner surface 11a to the bottom surface 11b facing the raw material inlet 14, which is tapered in cross section and spiral in plan view. It is formed in a shape.

  Since the accommodating portion 20 enlarged by the tapered passage 11c is formed at the lower end portion of the raw material inlet 14, the cellulose-containing raw material introduced into the raw material inlet 14 enters the gap 13 and is sheared and crushed. Immediately before entering the housing portion 20, the upper die 11 is cooled by heat radiation from the inner surface 11 a of the upper die 11 cooled by the antifreeze liquid circulated from the thermostat 29 inside the upper die 11 or heated by the heater 17. It is heated by heat transfer from the inner surface 11a. In addition to the above method, the apparatus 10 can be heated and cooled by installing the Peltier element 17 on the upper mill 11 as described above.

  The above-described thermocouple is inserted into a hole formed from the side surface of the upper die 11 toward the center, and approximately shows the processing temperature when being sheared and ground in the gap 13 between the upper die 11 and the lower die 12. ing. On the surface facing the gaps 13 of the upper mill 11 and the lower mill 12, a plurality of concave grooves extending in the direction intersecting the circumferential direction are formed in order to increase the shearing force on the cellulose-containing raw material.

  Next, the cellulose amorphization process performed using this apparatus 10 will be described. First, the gap 13 between the upper mill 11 and the lower mill 12 is appropriately adjusted via the gap adjusting unit 16 according to the cellulose-containing raw material, the size of the pulverized material after the treatment, and the like.

  Further, an antifreeze liquid is circulated through the upper die 11 from a constant temperature bath 29 having a predetermined temperature, and the upper die 11 is cooled by heat conduction. Alternatively, the heater 17 is heated by the temperature controller 19 to a predetermined temperature (for example, can be set in increments of 10 ° C. within a range of 80 to 240 ° C.), and the upper die 11 is heated by the heat conduction.

  Further, the motor 15 is driven at a rotation speed controlled by the computer 22 to rotate the lower mill 12 so as to give a predetermined shear rate.

  Since the preparation of the apparatus 10 is completed as described above, the cellulose-containing raw material is charged into the charging port 14 and processing is started.

  In the case of heat removal pulverization, since the upper mill 11 is cooled by the circulation of the antifreeze liquid from the thermostat 29, the cellulose-containing raw material passes through the inlet 14 and further passes through the tapered passage 11 c or the accommodating portion 20. Then, it is cooled to a temperature corresponding to the temperature of the antifreeze, and immediately thereafter, it is fed into the gap 13 between the lower die 12 and crushed by receiving a shearing force between the fixed upper die 11 and the rotating lower die 12. Is done.

  In the case of heat pulverization, the heater 17 has already been heated to a predetermined temperature, and thus the upper die 11 is also heated, so that the cellulose-containing raw material passes through the heater 17 and the inlet 14 and further tapers 11c through 11c. While passing through the housing portion 20, it is heated to a temperature corresponding to the heater temperature, and immediately after that, it is fed into the gap 13 between the lower die 12 and between the fixed upper die 11 and the rotating lower die 12. It is crushed by receiving shearing force.

  The powder containing amorphous cellulose obtained by shearing and pulverizing is discharged from the side of the gap 13 and accommodated in the receiving tray 26, and is collected in a predetermined container (not shown) through the dropping port 27 and the dropping chute 28. The

  The apparatus shown in FIGS. 1 and 2 is only an example that can be used for carrying out the method of the present invention, and any other apparatus can be used as long as it can carry out the method of the present invention. Also good.

In the present invention, “pulverizing a cellulose-containing raw material by applying a shearing force” includes an embodiment including the following conditions (i) to (iii).
(i) Two members that steadily move relative to each other (mainly steady relative rotation, other parallel translation, etc.). In particular, “steady relative movement” includes relative movement of members at a rotational speed and movement speed controlled in an apparatus manner.
(ii) A minute gap between two members.
(iii) Application of shearing force to the cellulose-containing raw material introduced into the gap by sliding of the member under steady surface pressure or linear pressure by the two members.
For example, as a device for applying a shearing force to a cellulose-containing raw material and crushing, the raw material grain is passed through a fine gap between two relatively rotating rollers in addition to the illustrated mortar device used in the embodiment. An apparatus configuration that shears and pulverizes in between, a small-diameter cylindrical or columnar member and a large-diameter cylindrical member are concentrically arranged and rotated relative to each other so that a minute amount between the outside of the small-diameter member and the inside of the large-diameter member An apparatus configuration that shears and pulverizes the raw grain through the gap can be used.

  The surface facing the gap between these rotating members (the mortar used in the examples, the above-mentioned roller, the small-diameter cylindrical or cylindrical member and the large-diameter cylindrical member, etc.) has a shearing force on the cellulose-containing raw material. From the point of increasing, it is preferable that a plurality of concave grooves extending in a direction intersecting the circumferential direction is formed.

  These aspects are distinguished in Patent Documents 1 and 2 from the technique of amorphizing a cellulose-containing raw material by vibration using a medium or the like, and are derived from crystals by heat removal pulverization as seen in Examples described later. The diffraction peak is significantly reduced and low crystallinity is exhibited.

  Although the time of a shearing process is not specifically limited, From a viewpoint of reducing a crystallinity degree, a shearing process can be performed in 0.01 to 10 hours, for example. However, in the present invention, the shearing process can be performed in a remarkably short processing time as compared with the technique using a ball mill or the like as in Patent Documents 1 and 2, and typically in about 10 to 60 seconds. .

  The degree of crystallinity of the amorphous cellulose obtained by the present invention is preferably less than 50%, more preferably 45% or less, even more preferably 30% or less, and particularly preferably 20% or less in consideration of utilization of industrial materials and the like. .

  The average particle size of the non-crystalline cellulose-containing pulverized product obtained by the present invention is, for example, 10 to 40 μm.

  In addition, the non-crystallized sample subjected to the pulverization treatment of the present invention clearly has improved saccharification characteristics as compared with the untreated or heat-pulverized sample (FIGS. 13 and 14). Therefore, the non-crystallized sample which performed the grinding | pulverization process of this invention is excellent also in the saccharification characteristic important in manufacturing bioethanol. In conventional saccharification, cellulose is treated with an organic solvent to reduce the crystallinity of cellulose and increase saccharification, but the amorphous technology of the present invention only pulverizes under temperature-controlled conditions. It is possible to improve saccharification.

  Amorphous cellulose obtained by the present invention can be expected to be used in a wide range of industrial fields such as bioethanol, food, and plastic additives.

  EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.

The crystallinity, water content, and average particle size of the cellulose-containing raw material or non-crystalline cellulose were measured by the following methods.
(1) Crystallinity Cellulose I type crystallinity is calculated by the Segal method from the diffraction intensity value by the X-ray diffraction method, and is defined by the following equation.

Cellulose type I crystallinity (%) = [(I 22.6−I 18.5) / I 22.6] × 100
[I 22.6 indicates the diffraction intensity of the lattice plane (002 plane) (diffraction angle 2θ = 22.6 °) in X-ray diffraction, and I 18.5 indicates the diffraction intensity of the amorphous portion (diffraction angle 2θ = 18.5 °). ]
Cellulose type I crystallinity was calculated from the above equation by measuring the X-ray diffraction intensity of a sample using “RINT2200” manufactured by Rigaku Corporation under the following conditions.
X-ray source: Cu / Kα-radiation
Tube voltage: 40kv
Tube current: 30mA
Measurement range: Diffraction angle 2θ = 5-35 °
X-ray scanning speed: 10 ° / min
(2) Moisture content Moisture content is measured with a moisture meter (Kett, product name: FD-720).
Measurement was performed using
(3) Average particle size The shape and particle size of the sample before and after pulverization were evaluated using a laser microscope and a laser diffraction particle size distribution analyzer (Mastersizer 2000 manufactured by Malvern).
<Example 1>
Using a piece of cypress wood as a raw material, shearing was performed using the apparatus 10 having the configuration shown in FIGS. 1 and 2.

  In the apparatus 10 used, the upper mortar 11, the lower mortar 12 and the heater 17 all have an outer diameter of 50 mm (radius 25 mm), and have an inlet 14 having a diameter of 10 mm at the center.

  The tapered raw material passage 11c of the upper mill 11 is formed over a range of 5 mm from the inner surface 11a (FIG. 2). The gap 13 between the mortars was set to 0.01 mm, and shearing was performed at a pulverization temperature (the above-described thermocouple measurement temperature; the same applies to the following examples) at −10 to 240 ° C. The rotational speed of the lower mill 12 was 80 rpm.

  The result of this shearing process is shown in the wide-angle X-ray diffraction graph of FIG.

  From this graph, the heat pulverization (80 to 240 ° C.) showed no change in the diffraction peak and showed the same high crystallinity as that of the untreated. Also, even when pulverized under a cooling condition of −10 ° C., no change was observed in the diffraction peak, and the same high crystallinity as that in the untreated state was exhibited.

  However, it was found that by performing heat removal pulverization (0 to 15 ° C.), the diffraction peak is remarkably reduced and low crystallinity is exhibited.

  Furthermore, it was found that fine pulverization and low particle size appeared more significantly than other pulverization conditions by heat removal pulverization (FIG. 4).

From the above, it was found that by removing heat and pulverizing, cellulose can be made into a fine powder and the crystallinity can be remarkably reduced.
<Example 2>
The water content of the cypress wood pieces was changed, and the pulverization treatment was performed under the same conditions as in Example 1 except that.

The results are shown in the wide-angle X-ray diffraction graph of FIG. 5 ((a) has a water content of about 1% by weight and (b) has a water content of about 20% by weight). The dried sample (water content about 1% by weight) showed a decrease in the peak derived from the crystals.
<Example 3>
The rotational speed of the lower mill 12 was changed in the range of 80 to 380 rpm, and the pulverization treatment was performed under the same conditions as in Example 1 except that.

The results are shown in the wide-angle X-ray diffraction graph of FIG. 6 ((a) is heat removal pulverization (15 ° C.), (b) is heat pulverization (140 ° C.)). In the sample subjected to heat removal grinding (15 ° C.) and ground at a low rotational speed, a decrease in the diffraction peak derived from the crystal was observed.
<Example 4>
Hinoki wood pieces were infiltrated with ethanol for 24 hours and used as raw materials. Otherwise, the pulverization treatment was performed under the same conditions as in Example 1.

The results are shown in the wide-angle X-ray diffraction graph of FIG. From the results shown in FIG. 7, it was found that even when the sample was impregnated with ethanol before pulverization, the heat-induced pulverization (15 ° C.) reduced the crystal-derived diffraction peak significantly and exhibited low crystallinity. On the other hand, in the heat pulverization (80 to 200 ° C.), no change was observed in the diffraction peak, and the same high crystallinity as that of the untreated was shown.
<Example 5>
A commercially available high-purity crystalline cellulose fiber (CF11 manufactured by Whatman, crystallinity 85.7%) was used as a raw material, and pulverization was performed under the same conditions as in Example 1. Unlike the wood pieces used in Examples 1 to 4, this sample does not substantially contain lignin and has high cellulose purity.

  The results are shown in FIGS. FIG. 8 is a wide-angle X-ray diffraction graph, FIG. 9 is a graph showing the relationship between the pulverization temperature and the cellulose crystallinity of the pulverized product, and FIG. 10 is a measurement result of the particle size distribution of cellulose after pulverization according to the pulverization temperature. FIG. 11 is a graph (left) and a photograph (right) showing the relationship between the pulverization temperature and the particle size distribution of the cellulose after pulverization. The graph (left) and the photograph (right) show samples corresponding to (a), (b), and (c), respectively.

From these graphs, in the same manner as in Example 1, by carrying out heat removal pulverization (15 ° C.), even in crystalline cellulose fibers having a high cellulose purity, the diffraction peak derived from the crystals is remarkably reduced by the pulverization treatment, resulting in low crystallinity. I found out that The crystallinity decreased from 85.7% to 20.1%. On the other hand, in the heat pulverization (80 to 240 ° C.), no change was observed in the diffraction peak, and the same high crystallinity as that of the untreated was shown. FIG. 9 shows that the crystallinity has a clear correlation with temperature (heating, heat removal). In addition, it has been clarified that low crystalline cellulose can be obtained by removing heat from both wood chips and high purity crystalline cellulose. (Fig. 3, Fig. 8)
Furthermore, it was found that fine pulverization and low particle size appeared more significantly than other pulverization conditions by heat removal pulverization (FIGS. 10 and 11).
<Example 6>
A commercially available high-purity crystalline cellulose fiber (CF11 manufactured by Whatman, crystallinity 85.7%) was used as a raw material, and pulverization was performed under the same conditions as in Example 1. Similar to Example 5, this sample contains almost no lignin and has high cellulose purity.

  In this example, the periphery around the upper side of the temperature range of the heat removal pulverization, which was clearly different from the heat pulverization (80 to 240 ° C.) in Examples 1 to 5 and the crystal-derived diffraction peak significantly decreased and showed low crystallinity ( (10 ° C, 15 ° C, 20 ° C, 30 ° C, 40 ° C, 60 ° C).

  The results are shown in the wide-angle X-ray diffraction graph of FIG.

From this graph, the crystal-derived diffraction peak tends to decrease when the temperature is below 40 ° C, and the critical peak is 30 ° C or less, especially at 25 ° C or less. It was found to show low crystallinity.
<Example 7>
Using cedar and beech wood as raw materials, pulverization was performed under the same conditions as in Example 1 except that the saccharification characteristics by cellulase were evaluated. FIG. 13 shows saccharification characteristics of cedar and FIG. 14 shows saccharification characteristics of beech. The graph shows the time course of the glucose concentration under each condition of untreated, 15 ° C. grinding, and 140 ° C. grinding.

  The sample subjected to the amorphization treatment by heat removal pulverization (15 ° C.) clearly has improved saccharification characteristics as compared with the untreated sample and the heat pulverization (140 ° C.) sample. Thus, the amorphous treatment by heat removal pulverization is also excellent in saccharification characteristics that are important in producing bioethanol.

DESCRIPTION OF SYMBOLS 10 Milling device 11 Upper mill 11a Inner surface 11b Bottom surface 11c Tapered raw material path 12 Lower mill 13 Gap 14 Raw material inlet 15 Motor 16 Gap adjustment part 17 Heater (or Peltier element)
18 Heater code 19 Temperature controller 20 Housing part 21 Data cable 22 Computer 23 Data cable 24 Temperature control cable 25 Motor control cable 26 Receptacle 27 Drop port 28 Drop chute 29 Constant temperature bath

Claims (4)

A process for producing amorphous cellulose, comprising a step of subjecting a cellulose-containing raw material to a heat removal pulverization by applying a shearing force under a temperature condition of -5 to 25 ° C. to make the cellulose amorphous. The method for producing amorphous cellulose according to claim 1 , wherein the cellulose-containing raw material is a piece of wood. The method for producing amorphous cellulose according to claim 1 or 2 , wherein the cellulose-containing raw material having a water content of 0.5 to 20% by mass is subjected to shear removal by applying a shearing force. The non- heat pulverized product according to any one of claims 1 to 3, wherein the gap between two relatively moving members is set to 0.5 mm or less, and a cellulose-containing raw material is put into the gap to apply a shearing force to remove heat. A method for producing crystallized cellulose.