JP2016030240A - Method for producing powdered cellulose - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a vibration pulverizer and a method for producing a powdered cellulose where the powdered cellulose can be efficiently produced from a chip-formed cellulose-containing raw material and productivity is excellent.SOLUTION: A vibration pulverizer 100 is provided with: a container 1 having a raw material charge port 11 and a discharge port 12, having a columnar space inside, being disposed so that the central axis of the columnar space becomes nearly horizontal and being held so as to be able to vibrate in an in-plane direction nearly perpendicular to the central axis; and a plurality of cylindrical media disposed so as to be able to vibrate in a central axis direction at the inside of the container and made of two kinds of cylindrical media 2A, 2B. A method for producing a powdered cellulose in the vibration pulverizer 100 satisfying specific conditions, includes a step that a chip-formed cellulose-containing raw material is introduced to the inside of the container of the vibration pulverizer 100 from the raw material charge port and pulverized by vibrating the container and then the obtained powdered cellulose is discharged from the discharge port.SELECTED DRAWING: Figure 1

Description

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

It is generally well known that by reducing the particle size of a substance to increase the specific surface area, the reactivity of the substance is improved and properties relating to handling properties such as bulk density are changed. In the method of reducing the particle size of a substance, one of the most basic unit processes is a pulverization process. In the old days, minerals and inorganic substances such as calcium carbonate are pulverized. Very diverse.
In addition, substances having a crystal structure generally have poor reactivity and are difficult to use. In certain milling processes, it becomes possible to amorphize the material simultaneously with milling, and its reactivity can be significantly improved. As a result, various functional groups can be bonded to the amorphous material by a chemical reaction, and the value can be dramatically increased.

  In recent years, biomass materials have attracted attention due to growing awareness of environmental issues. Cellulose-containing raw materials such as cellulose ethers and cellulose derivatives are used as raw materials for cellulose derivatives such as cellulose ethers and cosmetics. It is used for industrial raw materials such as food and biomass materials. Various pulverizers used for pulverizing the cellulose-containing raw material have also been proposed.

For example, Patent Document 1 discloses a container having a cylindrical space inside and a cylindrical medium, and pulverized inside the cylindrical medium for the purpose of reducing the particle size of the raw material in a short time and improving productivity. A method for producing a pulverized product using a specific vibration pulverizer equipped with a medium is disclosed.
In Patent Document 2, as a pulverizer for atomization, a rotating body in which a plurality of convex portions are formed in a cylindrical container and an axial hole is formed in the center is inserted as a pulverizing medium. An apparatus for revolving and pulverizing woody biomass is disclosed.
In Patent Document 3, as a pulverizer for atomization, an apparatus for pulverizing woody biomass by inserting a plurality of thick discs with protrusions into a cylindrical container as a pulverizing medium and vibrating the cylindrical container up and down Is disclosed.
In Patent Document 4, for the purpose of efficiently obtaining a high-purity pulverized product, a disc ring-type pulverization for a high-purity pulverized product loaded with an end plate and a disc ring-type pulverization medium having a smooth outer circle surface. A medium-use vibration mill is disclosed.

JP2013-139018A JP 2009-233542 A JP 2008-93590 A JP 2012-11331 A

  As described above, it is possible to finely pulverize an object to be pulverized such as cellulose by a pulverizer using a ring-shaped pulverizing medium. In a pulverizer using a ring-shaped pulverizing medium, a material to be pulverized is introduced into a gap between the pulverizing medium and a container in which the pulverizing medium is stored, and a gap between the pulverizing media. Then, the object to be crushed is pulverized by utilizing the collision between the pulverizing media. However, since the gap is usually narrow, the pulverizer may be clogged with the pulverized material when a large amount of pulverized material is pulverized or when the supply speed of the pulverized material is high. Therefore, when a large amount of materials to be pulverized is pulverized rapidly, a more efficient method is required than the pulverization method using the pulverizer described in Patent Documents 1 to 4.

  This invention makes it a subject to provide the manufacturing method of the vibration crusher excellent in productivity which can manufacture powdered cellulose efficiently from a chip-shaped cellulose containing raw material, and powdered cellulose.

The present inventors have a raw material inlet and a discharge port, have a cylindrical space inside, and are arranged so that a central axis of the cylindrical space is substantially horizontal, and substantially perpendicular to the central axis. A container that can be vibrated in an in-plane direction, and at least two kinds of cylindrical media of a predetermined shape that are arranged in the container so as to vibrate in the direction of the central axis. It has been found that the above problem can be solved by using a vibration pulverizer that satisfies the conditions.
That is, the present invention provides the following [1] and [2].
[1] Provided with a raw material input port and a discharge port, have a cylindrical space inside, and are arranged so that the central axis of the cylindrical space is substantially horizontal, and in a plane substantially perpendicular to the central axis And a plurality of cylindrical media arranged in the central axis direction so as to be able to vibrate. The plurality of cylindrical media are two types of cylindrical media A. And a vibration pulverizer comprising the cylindrical medium B and satisfying the following conditions (1) to (4).
(1) The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container.
(2) a cylindrical medium B, it 70mm or more in length in the central axial direction when the 110mm or less, the opening area 25 cm ² or more on the outer peripheral side surface, has at least one 250 cm ² or less of the opening, and the opening The ratio of the sum of the opening areas to the total area of the outer peripheral side surface including the portion is 10% or more and 50% or less.
(3) The cylindrical medium B is disposed so that the central axis thereof is substantially parallel to the central axis of the columnar space inside the container, and at least one cylindrical medium B satisfies the following formula: Placed in.
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance parallel to the central axis (4) The average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less.
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)
[2] A method for producing powdered cellulose in which a chip-like cellulose-containing raw material is pulverized using the vibration pulverizer according to [1], wherein the cellulose-containing raw material is introduced into the container of the vibration pulverizer. A method for producing powdered cellulose, comprising the steps of introducing the powdered cellulose, pulverizing the container by shaking, and discharging the obtained powdered cellulose from the outlet.

  According to the vibration pulverizer of the present invention and the method for producing powdered cellulose using the vibration pulverizer, the chip-shaped cellulose-containing raw material can be introduced into the vibration pulverizer without clogging. Therefore, even if the feed rate of the raw material is high, powdered cellulose having a reduced particle size can be efficiently produced without causing clogging.

It is a mimetic diagram showing an example of a vibration crusher of an embodiment of the present invention. 3 is a schematic diagram illustrating an example of a cylindrical medium A. FIG. 3 is a schematic diagram illustrating an example of a cylindrical medium B. FIG. It is a perspective view which shows an example which used the cylindrical rod-shaped medium as a grinding | pulverization medium further in the vibration grinding machine of embodiment of this invention.

[Vibrating crusher]
The vibration pulverizer according to the present invention includes a raw material inlet and an outlet, has a cylindrical space inside, and is arranged so that a central axis of the cylindrical space is substantially horizontal, with respect to the central axis. A container that is held so as to be able to vibrate in a substantially vertical in-plane direction, and a plurality of cylindrical media that are arranged so as to be able to vibrate in the central axis direction are provided inside the container. And the following conditions (1) to (4) are satisfied.
(1) The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container.
(2) a cylindrical medium B, it 70mm or more in length in the central axial direction when the 110mm or less, the opening area 25 cm ² or more on the outer peripheral side surface, has at least one 250 cm ² or less of the opening, and the opening The ratio of the sum of the opening areas to the total area of the outer peripheral side surface including the portion is 10% or more and 50% or less.
(3) The cylindrical medium B is disposed so that the central axis thereof is substantially parallel to the central axis of the columnar space inside the container, and at least one cylindrical medium B satisfies the following formula: Placed in.
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance parallel to the central axis (4) The average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less.
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)

The vibration crusher of this invention is demonstrated using FIGS.
An example of an embodiment of the vibration pulverizer of the present invention is shown in FIG. FIG. 1A is a schematic cross-sectional view of a vibration pulverizer in the direction of the central axis of a container arranged so as to be substantially horizontal, and FIG. 1B is a diagram of the vibration pulverizer with respect to the central axis. It is the schematic diagram seen from the perpendicular in-plane direction.
A vibration crusher 100 shown in FIG. 1 includes a raw material inlet 11 and an outlet 12, has a cylindrical space inside, and is arranged so that a central axis of the cylindrical space is substantially horizontal, A container 1 held so as to be able to vibrate in an in-plane direction substantially perpendicular to the central axis of a cylindrical space, and a plurality of cylindrical media arranged in the container 1 so as to vibrate in the direction of the central axis. Prepare. A plurality of cylindrical media are arranged in the central axis direction (hereinafter also simply referred to as “axial direction”) of the columnar space. In FIG. 1, the holding portion of the container 1 is not shown.
Here, the plurality of cylindrical media are composed of two types of cylindrical media, that is, cylindrical media A (2A in FIGS. 1 and 2) and cylindrical media B (2B in FIGS. 1 and 3). The medium 2B has an opening 21 defined by the condition (2). FIG. 1A shows a mode in which a plurality of cylindrical media 2A are provided and only one cylindrical media 2B is provided, but the present invention is not limited to this mode. In the description relating to the drawings in this specification, the cylindrical medium 2A and the cylindrical medium 2B may be collectively referred to as “cylindrical medium 2”.

As shown in FIG. 4, the vibration pulverizer 100 of the present invention may include a pulverizing medium 3 disposed in a cylindrical medium 2 (inside space) so as to be further vibrated. Examples of the grinding medium 3 used in the present invention include a rod-shaped medium and a spherical medium, and these may be used in combination. FIG. 4 shows a mode in which a plurality of cylindrical rod-shaped media are provided as the grinding media 3.
In FIG. 4, in order to display the cylindrical medium 2 and the pulverizing medium 3 disposed inside the container 1, a part including the raw material input port 11 and the discharge port 12 of the container 1 and the holding unit of the container 1 are omitted. Is shown.

In the vibration pulverizer of the present invention, the chip-like cellulose-containing raw material can be introduced into the vibration pulverizer without clogging, and the reason why powdered cellulose can be produced efficiently is not clear, but is considered as follows.
In the vibration pulverizer of the present invention having a cylindrical medium inside the container, the cylindrical medium rotates at high speed inside the container, and the gap between the cylindrical medium and the container and the gap between the cylindrical media are pulverized. The product (chip-shaped cellulose-containing raw material) passes through and is pulverized. Here, in order to finely pulverize the object to be crushed, it is necessary to narrow the gap between the cylindrical medium and the container and the gap between the cylindrical media to some extent. On the other hand, if these gaps are too narrow, the fluidity of the material to be crushed inside the container deteriorates, causing clogging or stagnation of the material to be crushed, making it impossible to introduce the material to be pulverized, and progressing powdering No longer.
The chip-shaped cellulose-containing raw material to be pulverized rotates along with rebounding between the cylindrical medium and the container. Here, in the present invention, a cylindrical medium B having a predetermined opening on the outer peripheral side surface is used as the cylindrical medium, and the predetermined opening is provided so that the opening of the cylindrical medium B is in the vicinity of the raw material inlet of the container. (Conditions (2) and (3)). For this reason, it is considered that the cellulose-containing raw material enters the cylindrical medium from the opening of the cylindrical medium B, the fluidity of the cellulose-containing raw material is improved, and the raw material is not blocked in the container.
The cylindrical medium B having an opening has a smaller contact area with the container than that having no opening. However, in the present invention, since the fluidity of the cellulose-containing raw material is further improved as described above, even when the cellulose-containing raw material moves from the inside of the cylindrical medium to the outside due to vibration and rotation of the cylindrical medium, Can pass through more gaps.
Since the cylindrical medium B is provided with an opening, it is necessary to increase the length in the direction of the central axis as compared with a medium without an opening, and therefore the number of cylindrical media B that can be disposed inside the container is limited. Moreover, since the weight is reduced by the amount of the opening, the vibration in the central axis direction is likely to occur during vibration. From the above points, when the cylindrical medium B is used, the contact area between the cylindrical media also decreases. Therefore, in the present invention, the average gap distance between the cylindrical media is set within a predetermined range (condition (4)). By narrowing the average gap distance to some extent, the vibration in the direction of the central axis during vibration of the cylindrical medium is reduced, and the number of contacts between the cylindrical media is increased to finely pulverize the object to be crushed. Can do. On the other hand, by increasing the average gap distance to some extent, it is possible to avoid deterioration of the fluidity, clogging and retention of the material to be crushed.
Therefore, in the present invention, by using the cylindrical medium B, it is possible to obtain powdered cellulose efficiently even though the contact area between the container and the cylindrical medium and the contact area between the cylindrical media are reduced. it is conceivable that.

<Container>
In the vibration pulverizer of the present invention, the container includes a raw material inlet and a discharge port, has a cylindrical space inside, and is arranged so that the central axis in a stationary state of the cylindrical space is substantially horizontal. And is held in a state capable of vibrating in an in-plane direction substantially perpendicular to the central axis. Here, the “center axis of the cylindrical space” means a virtual straight line passing through the center of gravity of the two circular bottom surfaces of the cylinder, and “substantially horizontal direction” means that the angle formed with the horizontal plane is −10 to −10. The direction is 10 ° (hereinafter, “substantially horizontal direction” is also simply referred to as “horizontal”). Although the material of a container is not specifically limited, For example, metals and alloys, such as iron, steel, and stainless steel, can be used and the process of hardening etc. may be performed.
The shape of the space inside the container is preferably a substantially circular cylindrical shape such as a perfect circle or an ellipse from the viewpoint of uniform pulverization.
The size of the container is not particularly limited. For example, the inner diameter of the container is preferably 50 mm or more, more preferably 80 mm or more, further preferably 100 mm or more, preferably 1500 mm or less, more preferably 1200 mm or less, and still more preferably 1000 mm or less. Further, the length in the central axis (hereinafter also referred to as “container axis”) direction of the cylindrical space inside the container is preferably 100 mm or more, more preferably 120 mm or more, further preferably 150 mm or more, and 10,000 mm or less. Is preferable, 8000 mm or less is more preferable, and 6000 mm or less is still more preferable. In the present invention, the inner diameter of the container means twice the shortest distance from the axis of the container to the inner surface of the container. When the bottom surface of the cylindrical space is a perfect circle, it is equal to the diameter of the perfect circle. When it is a shape, it is equal to the minor axis of the ellipse.

The container vibrates in an in-plane direction substantially perpendicular to the container axis when pulverized. The vibration of the container in the present invention does not only indicate a motion in which the locus of the axis of the container draws a straight line but includes a motion that draws an ellipse or a perfect circle.
The frequency and amplitude of the container are not particularly limited. By increasing the frequency and amplitude, the acceleration applied to the container, the cylindrical medium arranged inside the container, and the grinding medium arranged inside the cylindrical medium. And the pulverization rate of the cellulose-containing raw material can be increased.
Therefore, the frequency of the container is preferably 8 Hz or more, more preferably 10 Hz or more, and further preferably 12 Hz or more. The amplitude of the container is preferably 5 mm or more, more preferably 6 mm or more, and still more preferably 7 mm or more from the viewpoint of the grinding speed.
On the other hand, from the viewpoint of apparatus load, the frequency of the container is preferably 40 Hz or less, more preferably 35 Hz or less, and further preferably 30 Hz or less. Further, the amplitude of the container is preferably 25 mm or less, more preferably 20 mm or less, further preferably 18 mm or less, and further preferably 15 mm or less.
If the axis trajectory of the container does not draw a straight line, the container vibration has a plurality of amplitudes of different lengths. In the present invention, the container vibration amplitude is the longest amplitude of the container vibration amplitudes. For example, when the axis trajectory of the container draws an ellipse, it means the major axis of the ellipse.
The vibration mechanism of the container includes a vibration motor, an eccentric weight, an eccentric vibration device, or the like, and these mechanisms are the same as well-known mechanisms. The mechanism is disclosed in, for example, Japanese Patent Application Laid-Open No. 2008-93534, Japanese Patent Application Laid-Open No. 2008-132469, and the like in addition to the above-mentioned Japanese Patent Application Laid-Open No. 2004-188833.

Introduction of the chip-shaped cellulose-containing raw material into the container is performed by continuously supplying it from the raw material inlet while performing a pulverization process. As shown in FIG. 1A, the raw material inlet 11 is preferably provided at the upper part of the container, more preferably at the upper part of one end of the container, and the outlet 12 is preferably provided at the lower part of the end opposite to the raw material inlet 11. Prepare. Thereby, a continuous crushing process becomes possible. Normally, when the raw material inlet is provided in the upper part of the container, compared with the case where the raw material inlet is provided in the axial side surface of the container (the bottom part of the cylinder in the cylindrical space of the container). In addition, the cellulose-containing raw material is difficult to move into the cylindrical medium, and clogging with the raw material is likely to occur. On the other hand, the present invention is useful in that powder cellulose can be produced efficiently without clogging with the cellulose-containing raw material even when the raw material inlet is provided at the upper part of the container.
There are no particular restrictions on the cross-sectional shape of the raw material inlet and outlet, but it is preferably substantially circular. The inner diameters of the raw material inlet and outlet are not particularly limited as long as they are equal to or smaller than the inner diameter of the container. In the present invention, the inner diameter of the raw material inlet (or outlet) means twice the shortest distance from the central axis of the raw material inlet (or outlet) to the inner surface of the raw material inlet (or outlet).
The raw material inlet and outlet may be provided directly in the container, or may be connected to the container via other members. In the vibration crusher 100 shown in FIG. 1A, the raw material inlet 11 is directly provided at the upper part of one end of the container, and the outlet 12 is opposite to the raw material inlet 11 of the container 1 through the lid portion 13. It is connected to the lower part of the side end.
In the connection portion between the discharge port 12 and the container 1, in order to allow the cellulose-containing raw material to stay in the container 1 and to perform sufficient pulverization, the cylindrical shape of the container 1 is placed inside the container 1 near the discharge port 12. The amount of discharge may be limited by providing a weir so as to be parallel to the bottom surface of the cylinder in the space. For example, in the vibration crusher of FIG. 1A, a weir can be provided on the boundary surface between the lid 13 and the container 1.

The vibration pulverizer of the present invention may have two containers of the same shape in the upper and lower sides. In this case, the discharge port of the upper container and the raw material input port of the lower container are connected, and the chip-like cellulose-containing raw material introduced from the upper raw material input port is pulverized in the upper container After that, it is introduced into the lower container through the upper container outlet and the lower container raw material inlet, and is further pulverized in the lower container, and the lower container outlet Discharged from.
When the vibration pulverizer of the present invention is in the above-described embodiment, it is sufficient that at least one of the upper side and the lower side and the cylindrical medium disposed in the container satisfy the requirements of the present invention. In the vibration pulverizer of the present invention, it is preferable that at least the upper container and the cylindrical medium disposed inside the container satisfy the requirements of the present invention.

A cooling jacket may be attached around the container, and cooling may be performed during pulverization. Further, a nozzle for performing a nitrogen purge or the like may be provided in the upper part of the container near the material inlet and / or outlet of the container.
In order to prevent damage in the container due to collision between the container and the cylindrical medium, a cylindrical or curved steel plate may be inserted into the container as a lining. Even when the lining is damaged by the collision between the lining and the cylindrical medium, the lining can be easily replaced, which is preferable from the viewpoint of apparatus maintenance. The thickness of the lining is not particularly limited, but is preferably 1 mm or more, more preferably 3 mm or more, and further preferably 5 mm or more from the viewpoint of durability. Moreover, Preferably it is 30 mm or less, More preferably, it is 20 mm or less, More preferably, it is 16 mm or less.
As the vibration pulverizer equipped with the container as described above, a continuous vibration mill (such as “YAMT-50” manufactured by Eurus Techno Co., Ltd.), a vibration mill (manufactured by Chuo Kako Co., Ltd., etc.), a vibro mill (manufactured by Eurus Techno Co., Ltd.) ] Etc. are mentioned.

<Cylindrical medium>
In the vibration pulverizer of the present invention, as shown in FIGS. 1 and 4, the cylindrical medium is substantially parallel to the axis of the container and the central axis of each cylindrical medium (hereinafter also referred to as “the axis of the cylindrical medium”). In this state, a plurality of vibrations are arranged inside the container so as to vibrate in the axial direction of the container.
The cylindrical medium has a columnar space inside a column having a circular bottom surface, and has a so-called donut shape. Here, the “axis of the cylindrical medium” means a virtual straight line passing through the centers of the two substantially circular bottom surfaces of the columnar space inside the cylindrical medium. “Vibrating arrangement” means that when a container is vibrated, the cylindrical medium is arranged in a plane direction perpendicular to the axis of the container in the container and in a state capable of vibrating in the axial direction. Say.
In the vibration pulverizer of the present invention, the cylindrical medium vibrates inside the container by vibrating the container. Due to the vibration of the cylindrical medium, the cellulose-containing raw material passing through the gap between the container and the cylindrical medium and the gap between the cylindrical medium and the cylindrical medium is pulverized. Furthermore, when using a grinding | pulverization medium like FIG. 4, the grinding | pulverization speed by the several grinding | pulverization medium arrange | positioned so that a vibration is possible inside a cylindrical medium also improves. Accordingly, the particle size of the chip-like cellulose-containing raw material can be reduced more efficiently. When the cellulose in the cellulose-containing raw material is crystalline, the cellulose can be reduced in crystallization at the same time as pulverization.

  Here, the plurality of cylindrical media provided in the vibration pulverizer of the present invention include two types of cylindrical media A (2A in FIG. 1 and FIG. 2) and cylindrical media B (2B in FIG. 1) described below. 3). In the following description, the descriptions common to the cylindrical medium A and the cylindrical medium B are collectively referred to as “cylindrical medium”.

[Cylindrical medium A]
The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container (condition (1 )).
FIG. 2 is a schematic diagram showing an example of the cylindrical medium A. As shown in FIG. The axial length (x in FIG. 2) of the cylindrical medium A is 3 mm or more, preferably 5 mm or more, and more preferably 10 mm or more from the viewpoint of securing strength. Further, from the viewpoint of increasing the number of cylindrical media installed inside the container and increasing the number of gaps between adjacent cylindrical media to improve the fluidity of the cellulose-containing raw material inside the container, the shaft of the cylindrical medium A The length in the direction is 100 mm or less, preferably 70 mm or less, and more preferably 50 mm or less.

  The cylindrical medium A preferably has no opening on the outer peripheral side surface. This is for increasing the contact area between the container and the cylindrical medium A and improving the grinding efficiency.

[Cylindrical medium B]
The cylindrical medium B has a length in the central axis direction of 70 mm or more and 110 mm or less, and has at least one opening having an opening area of 25 cm ² or more and 250 cm ² or less on the outer peripheral side surface thereof, and includes the opening. The ratio of the sum of the opening areas to the total area of the outer peripheral side surface is 10% or more and 50% or less (condition (2)).
3A and 3B are schematic views showing an example of the cylindrical medium B. FIG. 3A is a perspective view of the cylindrical medium B, and FIG. 3B is a plan view viewed from the outer peripheral side surface direction of the cylindrical medium B. is there. The axial length of the cylindrical medium B (y in FIG. 3B) is 70 mm or more, preferably 75 mm or more, and preferably 80 mm or more from the viewpoint of securing strength while providing an opening in the cylindrical medium B. Is more preferable. In addition, if the weight of the cylindrical medium B is too heavy, the axial length of the cylindrical medium B is 110 mm or less, preferably 100 mm or less, and preferably 95 mm or less from the viewpoint of preventing the rotation of the cylindrical medium B. More preferred.

As shown in FIG. 3, the cylindrical medium B has at least one opening 21 on the outer peripheral side surface thereof. The opening area per opening 21 is 25 cm ² or more, preferably 30 cm ² or more, more preferably 50 cm ² or more, and further preferably 70 cm ² or more. The opening area is 250 cm ² or less, preferably 230 cm ² or less, more preferably 200 cm ² or less. When the opening area is less than 25 cm ² , the effect of introducing the cellulose-containing raw material into the cylindrical medium is not sufficiently exhibited, and the raw material is blocked. On the other hand, when the opening area exceeds 250 cm ² , the strength of the cylindrical medium B becomes weak, and the cylindrical medium B may be damaged during operation.

  The ratio of the total opening area to the total area of the outer peripheral side surface including the opening of the cylindrical medium B (hereinafter also referred to as “opening area ratio”) is 10% or more. Preferably it is 20% or more, more preferably 30% or more. Moreover, the said ratio is 50% or less, Preferably it is 45% or less, More preferably, it is 40% or less. When the opening area ratio of the cylindrical medium B is less than 10%, the effect of introducing the cellulose-containing raw material into the cylindrical medium is not sufficiently exhibited, and the blocking by the raw material occurs. If the opening area ratio exceeds 50%, the strength of the cylindrical medium B becomes weak, and the cylindrical medium B may be damaged during operation.

  The number of openings in the cylindrical medium B may be one or more, and from the viewpoint of maintaining the strength of the cylindrical medium B, it is preferably 5 or less, more preferably 4 or less.

The shape of the opening of the cylindrical medium B is not particularly limited, and examples thereof include substantially circular shapes such as a perfect circle shape and an elliptical shape, and polygonal shapes such as a triangle, a quadrangle, and a hexagon. In the case of having two or more openings, from the viewpoint of achieving both uniform pulverization of the cellulose-containing raw material and high opening ratio and strength of the cylindrical medium B, the openings may have the same shape and size. preferable.
Further, the arrangement of the openings on the outer peripheral side surface of the cylindrical medium B is not particularly limited, but when two or more openings are provided, the cellulose-containing raw material is uniformly pulverized, and the cylindrical medium B has a high opening ratio and strength. From the viewpoint of achieving both, it is preferable that the outer peripheral side surface is evenly disposed.

  The opening of the cylindrical medium B is preferably located at least 10 mm inside from the end of the cylindrical medium B in the central axis direction, and more preferably located at least 15 mm inside. In FIG. 3B, the end in the central axis direction of the cylindrical medium B is indicated by z in FIG. 3B, and the shortest distance z1 from the end z to the opening 21 is 10 mm or more. Is preferred. When the distance z1 is 10 mm or more, the occurrence of distortion due to heat during the processing of the cylindrical medium B having the opening is small, and the workability is good.

The cylindrical medium B is arranged so that the central axis thereof is substantially parallel to the central axis of the cylindrical space inside the container, and at least one cylindrical medium B is arranged at a position satisfying the following expression. (Condition (3)).
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance condition (3) parallel to the central axis will be described with reference to FIG. In FIG. 1A, a center line passing through the center of the opening 21 of the cylindrical medium 2B and perpendicular to the axial direction is 21B, a vertical center line passing through the center of the raw material inlet of the container is 11a, and a cylinder inside the container Of the ends in the central axis direction of the shape space, the vertical extension lines passing through the ends far from 11a are indicated by 12a. The longest distance d parallel to the central axis from the center of the raw material inlet of the container to the end corresponds to the distance between 11a and 12a in FIG. The cylindrical medium 2B is arranged such that the distance d1 between 11a-21B in FIG. 1A is a position of 0 ≦ d1 ≦ 0.3d.
The center of the raw material inlet means a contact point between the center of the cross section perpendicular to the moving direction of the raw material at the raw material inlet and the container. The center of the opening of the cylindrical medium B means the midpoint of the longest distance in the axial length of the opening provided in the cylindrical medium B.
In the vibration pulverizer of the present invention, the cellulose-containing raw material introduced from the raw material inlet is introduced into the cylindrical medium from the opening of the cylindrical medium B by disposing at least one cylindrical medium B at the above position. It can be easily introduced. For this reason, a cellulose containing raw material does not obstruct | occlude inside a container, and can manufacture powdered cellulose efficiently. When the center 21B of the opening of the cylindrical medium B is arranged at a position where the distance d1 from the raw material inlet center 11a exceeds 0.3d, the effect of introducing the cellulose-containing raw material into the cylindrical medium is sufficiently exhibited. Not blocked by the cellulose-containing raw material.
From the above viewpoint, the at least one cylindrical medium B is arranged such that the distance d1 is preferably in a position of 0 ≦ d1 ≦ 0.25d, more preferably 0 ≦ d1 ≦ 0.21d. Among these, from the viewpoint of promoting the amorphization of the cellulose-containing raw material, d1 is preferably 0.01 ≦ d1 ≦ 0.25d, more preferably 0.1 ≦ d1 ≦ 0.25d, and still more preferably 0.8. From the viewpoint of improving the processing amount, it is preferably 0 ≦ d1 ≦ 0.2d, more preferably 0 ≦ d1 ≦ 0.1d, and still more preferably 0. It arrange | positions so that it may become a position of <= d1 <= 0.05d.

In the vibration pulverizer of the present invention, the average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less (condition (4)).
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)
When the average gap distance exceeds 30 mm, unstable vibration in the axial direction occurs in the cylindrical medium B, so that the stable rotation of the cylindrical medium B is hindered and the pulverization efficiency is lowered. When the average gap distance is less than 0.1 mm, the chip-like cellulose-containing raw material is not smoothly supplied into the cylindrical medium, and the cellulose-containing raw material closes near the raw material inlet of the container. Therefore, continuous pulverization is difficult.
From the above viewpoint, the average gap distance is preferably 5.0 mm or less, and more preferably 1.0 mm or less. The average gap distance is preferably 0.2 mm or more, and more preferably 0.3 mm or more.
What is necessary is just to determine the number of cylindrical media so that the said conditions may be satisfy | filled.

  The total length in the central axis direction of the cylindrical medium is not particularly limited as long as it is shorter than the length in the central axis direction of the cylindrical space inside the container, but the contact area between the cylindrical medium and the container is increased and pulverized. From the viewpoint of increasing the speed, the ratio of the total length in the central axis direction of the cylindrical medium to the axial length of the cylindrical space inside the container (total length in the central axis direction of the cylindrical medium / container The axial length of the internal cylindrical space is preferably 0.80 or more, more preferably 0.85 or more, and still more preferably 0.90 or more. Further, it is preferably 0.995 or less, more preferably 0.99 or less, and still more preferably 0.98 or less.

The material of the cylindrical medium is not particularly limited. For example, metals such as iron, aluminum, steel, and stainless steel, alloys, and ceramics such as zirconia can be used. Stainless steel or steel may be subjected to a treatment such as quenching.
The shape of the cylindrical medium is such that when the cylindrical medium is vibrated inside the container, the kinetic energy due to the vibration of the container is efficiently transmitted to the cylindrical medium to improve the mobility of the cylindrical medium, and the cylinder From the viewpoint of increasing the collision energy when the pulverizing medium is present inside the cylindrical medium and increasing the number of collisions between the pulverizing media and between the cylindrical medium and the pulverizing medium, thereby improving the pulverization speed of the material to be pulverized. The cross-section of the inner space of the cylindrical medium is preferably a substantially circular shape such as a perfect circle or an ellipse, and a polygonal cylindrical shape having a hexagonal shape or more, and a perfect circular cylindrical shape is more preferable. Although there may be protrusions on the outer surface and the inner surface of the cylindrical medium, it is desirable that there are no protrusions from the viewpoint of preventing reduction in grinding efficiency due to wear of the cylindrical medium.

The difference between the inner diameter of the container and the outer diameter of the cylindrical medium in contact with the inside of the container (the inner diameter of the container−the outer diameter of the cylindrical medium) is preferably 3 mm or more, and more preferably 5 mm or more. 8 mm or more, more preferably 10 mm or more. Further, the difference from the outer diameter of the cylindrical medium in contact with the inside of the container is preferably 60 mm or less, more preferably 55 mm or less, further preferably 50 mm or less, and 45 mm or less. Is even more preferable. When the difference between the outer diameter of the cylindrical medium and the inner diameter of the container is within the above range, the pulverization rate of the cellulose-containing raw material can be increased. When the lining is inserted into the container, the value obtained by subtracting twice the length of the lining from the difference between the inner diameter of the container and the outer diameter of the cylindrical medium in contact with the container is within the above range. It is preferable to be within.
Further, from the viewpoint of increasing the contact frequency between the container and the cylindrical medium and increasing the pulverization rate of the cellulose-containing raw material, the ratio of the outer diameter of the cylindrical medium to the inner diameter of the container (the outer diameter of the cylindrical medium / the inner diameter of the container) is It is preferably more than 0.50, more preferably 0.70 or more, and still more preferably 0.80 or more. Further, from the viewpoint of easy vibration of the cylindrical medium inside the container, the ratio of the outer diameter of the cylindrical medium to the inner diameter of the container is preferably 0.95 or less, and more preferably 0.90 or less.

  In the present invention, the outer diameter of the cylindrical medium means twice the longest distance from the axis of the cylindrical medium to the outer surface of the cylindrical medium. For example, the outer peripheral shape of the cross section perpendicular to the axis of the cylindrical medium Means a diameter of a perfect circle, and if it is an ellipse, it means the major axis of the ellipse, and if it is a polygon, it is the longest of the distances from the center of gravity of the polygon to the vertex. Means twice as much.

From the viewpoint of the strength of the cylindrical medium, the ratio of the thickness of the cylindrical medium to the outer diameter of the cylindrical medium (thickness of the cylindrical medium / outer diameter of the cylindrical medium) is preferably 0.02 or more, and 0.03 The above is more preferable, and 0.05 or more is more preferable.
The ratio of the thickness of the cylindrical medium to the outer diameter of the cylindrical medium is preferably 0.7 or less from the viewpoint of promoting pulverization between the cylindrical media and improving the fluidity of the cellulose-containing raw material. 6 or less is more preferable, and 0.5 or less is still more preferable.
Especially when using grinding media, increase the amount of grinding media filled in cylindrical media, increase the number of collisions between grinding media and between cylindrical media and grinding media, and improve the grinding speed of raw materials to be ground. Can do.
Here, the “thickness of the cylindrical medium” means the thickness of a member that forms the cylindrical medium, and does not mean the axial length of the cylindrical medium. When the thickness of the cylindrical medium differs depending on the part, the thickness of the cylindrical medium means the thickness of the thickest part.
The length, thickness, inner diameter, outer diameter, shape, and material of the plurality of cylindrical media A are preferably the same. The same applies when a plurality of cylindrical media B are used.

<Crushing media>
As shown in FIG. 2, the vibration pulverizer of the present invention may have a mode in which a pulverizing medium is disposed inside a cylindrical medium so as to be able to vibrate. The shape of the grinding medium may be a cylindrical rod-shaped medium as shown in FIG. 4 or a spherical medium. Moreover, you may use combining these.
In the case where the vibration pulverizer of the present invention has two containers of the same shape in the upper and lower sides, an aspect in which the pulverization medium is provided only in one of the upper and lower containers may be used. An embodiment provided with a grinding medium may be used.
The material of the grinding medium is not particularly limited. For example, metals such as iron, aluminum, steel, and stainless steel, alloys, and ceramics such as zirconia can be used. The steel may be subjected to a treatment such as quenching.

Here, the integrated value of the volume of the grinding medium is preferably a value that exceeds 25% of the space volume inside the cylindrical medium in contact with the grinding medium.
In other words, the grinding medium is arranged inside the cylindrical medium so that the integrated value of the volume of the grinding medium exceeds 25% of the space volume inside the cylindrical medium in contact with the grinding medium. It is preferable that a plurality of the grinding media are arranged. When there are a plurality of grinding media, or when the integrated value of the volume of the grinding media (the sum of the volumes of the plurality of grinding media present in the container) exceeds 25% of the space volume inside the cylindrical media Therefore, the pulverization speed of the material to be pulverized is further improved.
The space volume inside the cylindrical medium is a columnar shape obtained by multiplying the area of the cross section perpendicular to the axis of the cylindrical medium by the length in the axial direction of the cylindrical medium. It refers to the space volume.

  From the viewpoint of increasing the number of collisions between the grinding media and between the cylindrical media and the grinding media to improve the grinding speed, the integrated value of the volume of the grinding media is 30% of the space volume inside the cylindrical media with which the grinding media are in contact. More preferably, it is more preferably 40% or more. Further, from the viewpoint of increasing the space for filling the cellulose-containing raw material and improving the productivity, the integrated value of the volume of the grinding medium may be 90% or less of the space volume inside the cylindrical medium in contact with the grinding medium. Preferably, it is 80% or less, more preferably 70% or less.

The shape of the rod-shaped medium is preferably a columnar shape or a polygonal prism having a quadrangle or more, more preferably a columnar shape, and a cross-section is a perfect circle from the viewpoint of suppressing wear due to collision with the cylindrical medium. More preferably, it has a certain columnar shape.
The outer diameter of the rod-shaped medium is preferably 3 mm or more, more preferably 5 mm or more, and even more preferably 7 mm or more from the viewpoint of increasing the impact force and improving the pulverization rate of the cellulose-containing raw material. . From the viewpoint of increasing the number of rod-shaped media, increasing the collision force and the number of collisions between the grinding media and between the cylindrical media and the grinding media to increase the grinding speed of the raw material to be ground, the outer diameter is 60 mm or less. Is preferably 50 mm or less, and more preferably 45 mm or less.
Here, the outer diameter of the rod-shaped medium means the length of a straight line that is on the cross section perpendicular to the length direction of the rod, passes through the center of gravity of the cross section, and has both ends on the outer periphery of the cross section. When it is a perfect circle, it means the diameter of the perfect circle.

The length of the rod-shaped medium is not particularly limited as long as it is shorter than the length in the central axis direction of the cylindrical space inside the container, but from the viewpoint of increasing the grinding speed by increasing the contact area between the cylindrical medium and the grinding medium, The ratio of the length of the rod-shaped medium to the axial length of the cylindrical space inside the container (the length of the rod-shaped medium / the axial length of the cylindrical space inside the container) is 0.80 or more. Preferably, it is 0.85 or more, more preferably 0.90 or more. Further, it is preferably 0.995 or less, more preferably 0.99 or less, and still more preferably 0.98 or less.
In order to facilitate maintenance of the apparatus, the rod-shaped medium may be divided into a plurality of pieces in the length direction.

  The outer diameter of the spherical medium is preferably 3 mm or more, more preferably 5 mm or more, and even more preferably 7 mm or more from the viewpoint of increasing the impact force and improving the grinding speed. Further, from the viewpoint of increasing the collision force of the spherical medium and the number of collisions between the grinding media and between the cylindrical medium and the grinding media and improving the grinding speed, the outer diameter is preferably 60 mm or less, and 50 mm or less. More preferably, it is more preferably 45 mm or less. The outer diameter of the spherical medium means the diameter of the sphere.

In the case of using a grinding medium, the vibration grinding machine of the present invention has a ratio of the inner diameter of the cylindrical medium in contact with the outer diameter of the grinding medium (the inner diameter of the cylindrical medium in contact with the grinding medium / the outer diameter of the grinding medium). (Diameter) is preferably 2.1 or more.
As shown in FIG. 2, the collision force and pulverization of the pulverization medium are arranged by arranging the plural pulverization media in a plane perpendicular to the axis of the cylindrical medium in the plurality of installed cylindrical media. By increasing the number of collisions between the media and between the cylindrical medium and the grinding medium, the grinding speed of the raw material to be ground can be improved. From the viewpoint of this grinding speed, the ratio of the inner diameter of the cylindrical medium in contact with the grinding medium to the outer diameter of the grinding medium (the inner diameter of the cylindrical medium in contact with the grinding medium / the outer diameter of the grinding medium) is 2.2 or more. More preferably, it is more preferably 2.5 or more. Further, the ratio of the inner diameter of the cylindrical medium in contact with the grinding medium to the outer diameter of the grinding medium is preferably 500 or less, more preferably 350 or less, further preferably 100 or less, and further preferably 50 or less. Is more preferable, and it is still more preferable that it is 25 or less.
In the present invention, the inner diameter of the cylindrical medium means twice the shortest distance from the axis of the cylindrical medium to the inner surface of the cylindrical medium.
Further, in the case of using the grinding medium, when the grinding medium comes out from the inside of the cylindrical medium when the container is vibrated, the vibration of the cylindrical medium inside the container is hindered. Therefore, it is preferable that the difference between the axial length of the cylindrical space inside the container and the axial length of the cylindrical medium is smaller than the axial length of the rod-shaped medium or the diameter of the spherical medium.

[Production method of powdered cellulose]
The method for producing powdered cellulose of the present invention is a method for producing powdered cellulose in which a chip-like cellulose-containing raw material is pulverized using the above-described vibration pulverizer of the present invention, and the chip-like cellulose-containing raw material is chip-shaped inside the container of the vibration pulverizer. A cellulose-containing raw material is introduced from the raw material inlet, and the container is vibrated and pulverized, and the obtained powdered cellulose is discharged from the outlet.

<Chip-like cellulose-containing raw material>
The cellulose-containing raw material used in the present invention is a chip-like cellulose-containing raw material from the viewpoint of continuous pulverization.
The cellulose-containing raw material to be crushed is not particularly limited. For example, various wood chips, various tree pruned branches, thinned wood, branch wood, building waste, factory waste, etc .; Examples include pulps such as wood pulp produced, and cotton linter pulp obtained from fibers around cotton seeds; papers such as cardboard, magazines, and fine paper.
The cellulose-containing raw material to be pulverized may be one of these, or may be a mixture of two or more. Among these, the cellulose-containing raw material to be pulverized is preferably pulps or woods, and more preferably pulps.

In the present invention, the chip-like cellulose-containing raw material pulverized by the vibration pulverizer may be subjected to a cutting process and / or a drying process, which will be described later, depending on the type and size of the raw material.
The shape of the chip-shaped cellulose-containing raw material is not particularly limited, and may be a cube, a rectangular parallelepiped, a granule, a rod, or the like. The size of the chip-shaped cellulose-containing raw material is preferably 10 mm or less, more preferably 7 mm or less, from the viewpoint of improving pulverization, the maximum value of the distance between any two points on the chip surface. More preferably, it is 5 mm or less. Further, from the viewpoint of processing into a chip shape, the minimum value of the distance between any two points on the chip surface is preferably 0.1 mm or more, more preferably 0.5 mm or more, and 1 mm or more. More preferably it is.

  In the cellulose-containing raw material used in the present invention, the cellulose content (α-cellulose content) in the remaining components obtained by subtracting water from the cellulose-containing raw material is preferably 20% by mass or more, and 40% by mass or more. More preferably, it is more preferably 60% by mass or more, still more preferably 70% by mass or more, and even more preferably 75% by mass or more. The upper limit of the α-cellulose content is 100% by mass. Here, the α-cellulose content can be measured by the method described in Examples.

The cellulose in a cellulose containing raw material consists of a crystalline region and an amorphous region. In the present invention, the cellulose I-type crystallization index is calculated by the Segal method from the diffraction intensity value by the X-ray diffraction method, and is defined by the following calculation formula (1). Specific measurement conditions for X-ray diffraction will be described in Examples.
Cellulose type I crystallization index (%) = [(I _22.6 −I _18.5 ) / I _22.6 ] × 100 (1)
[I _22.6 indicates the diffraction intensity of the lattice plane (002 plane) (diffraction angle 2θ = 22.6 °) of cellulose I-type crystal in X-ray diffraction, and I _18.5 indicates the amorphous part (diffraction angle 2θ = 18.5). °) shows the diffraction intensity. ]
Here, the cellulose type I is a crystalline form of natural cellulose, and the cellulose type I crystallization index means the ratio of the cellulose type I to the total amount of the crystalline region of cellulose.
There is no particular limitation on the cellulose I-type crystallization index of cellulose in the cellulose-containing raw material used as the material to be ground in the present invention. However, in general, the pulverization treatment for reducing the crystallization index of cellulose is accompanied by a decrease in the degree of polymerization due to breaking of the cellulose chain. From the viewpoint of obtaining powdered cellulose having a high average degree of polymerization and from the viewpoint of raw material costs, it is preferable to use a cellulose-containing raw material that is not exposed to the pulverization treatment for reducing the crystallization index as the cellulose-containing raw material. .
Therefore, the type I crystallization index of cellulose in the cellulose-containing raw material used as the material to be ground in the present invention is preferably more than 60%, more preferably 70% or more, and 75% or more. Further preferred.
On the other hand, since it is difficult to obtain a cellulose-containing raw material having a crystallinity index exceeding 95% and having a very high degree of crystallinity, the type I crystallization index of cellulose in the cellulose-containing raw material is preferably 90% or less. More preferably, it is 85% or less.

(Cutting process)
In the present invention, the chip-shaped cellulose-containing raw material pulverized by the vibration pulverizer can also be obtained by cutting the sheet-like cellulose-containing raw material. A method for cutting the cellulose-containing raw material in sheet form can be appropriately selected depending on the type of the cellulose-containing raw material and the size of the sheet. For example, one or more cutting machines selected from a shredder, a slitter cutter and a rotary cutter are used. However, it is preferable to use a shredder or a slitter cutter, and it is more preferable to use a slitter cutter from the viewpoint of productivity.
A slitter cutter is a cutting machine that cuts vertically with a roll cutter in the longitudinal direction along the longitudinal direction of the sheet to make an elongated strip shape, and then cuts it shortly along the width direction of the sheet with a fixed blade and a rotating blade. By using a slitter cutter, it is possible to easily obtain a cellulose-containing raw material having a dice shape. As a slitter cutter, a sheet pelletizer manufactured by Horai Co., Ltd., a super cutter manufactured by Hadano Seiki Seisakusho Co., Ltd. can be preferably used, and when these devices are used, a sheet-like cellulose-containing raw material is cut into about 1 to 20 mm square. can do. The thickness of the sheet-like cellulose-containing raw material sheet is preferably 0.1 mm or more and 3 mm or less from the viewpoint of cutting processability, although it depends on the performance of the cutting machine.

(Drying process)
The chip-shaped cellulose-containing raw material that has been subjected to the cutting treatment is preferably dried before being pulverized by a vibration pulverizer.
Generally, commercially available pulps contain water exceeding 5% by mass, and usually contain about 5-30% by mass of water. Therefore, in the present invention, from the viewpoint of improving the pulverization efficiency, it is preferable to adjust the water content of the cellulose-containing raw material to 9% by mass or less by performing a drying treatment, more preferably 4% by mass or less, and more preferably 3% by mass or less. Is more preferably 2% by mass or less, and particularly preferably 1% by mass or less. If this moisture content is 9% by mass or less, the grinding efficiency is improved. On the other hand, the lower limit of the moisture content is preferably 0.2% by mass or more, more preferably 0.3% by mass or more, and still more preferably 0.4% by mass or more, from the viewpoint of the productivity and drying efficiency of powdered cellulose. is there.
The water content can be measured by the method described in Examples.

The drying method may be appropriately selected from known drying means, for example, hot air heat receiving drying method, conductive heat receiving drying method, dehumidified air drying method, cold air drying method, microwave drying method, infrared drying method, sun drying method, A vacuum drying method, a freeze-drying method, etc. are mentioned.
In the above-mentioned drying method, a known dryer can be appropriately selected and used. For example, “Introduction to Powder Engineering” (Edited by the Powder Technology Information Center 1995, published by the Japan Society of Powder Technology) 176 pages And the like.
These drying methods and dryers may be used alone or in combination of two or more. The drying process can be either a batch process or a continuous process, but a continuous process is desirable from the viewpoint of productivity.
The continuous dryer is preferably a conductive heat receiving horizontal stirring dryer from the viewpoint of heat transfer efficiency. Furthermore, a biaxial horizontal stirring dryer is preferable from the viewpoint of the generation of fine powder and the stability of continuous discharge. As the biaxial horizontal stirring dryer, a biaxial paddle dryer manufactured by Nara Machinery Co., Ltd. can be preferably used.

  The temperature in the drying process cannot be determined unconditionally depending on the drying means, drying time, etc., but is preferably 10 ° C or higher, more preferably 25 ° C or higher, further preferably 50 ° C or higher, preferably 250 ° C or lower, and 180 ° C or lower. More preferred is 150 ° C. or lower. The drying treatment time is preferably 0.01 hours or more, more preferably 0.02 hours or more. Moreover, 2 hours or less are preferable and 1 hour or less are more preferable. If necessary, the drying treatment may be performed under reduced pressure. When the drying treatment is performed under reduced pressure, the pressure is preferably 1 kPa or more, more preferably 50 kPa or more, preferably 120 kPa or less, and more preferably 105 kPa or less.

(Crushing process)
After performing the cutting process, the chip-shaped cellulose-containing raw material subjected to the drying process as necessary is pulverized by the vibration pulverizer of the present invention. In the present invention, this may be referred to as “grinding treatment”.
Specifically, chip-like cellulose-containing raw material, which is a raw material to be crushed, is introduced into the container of the vibration pulverizer of the present invention from the raw material inlet, and pulverized by vibrating the container to obtain the obtained cellulose powder Is discharged from the outlet of the vibration crusher.
The frequency and amplitude of the container at the time of the pulverization treatment, and preferred ranges thereof are the same as those described in the section of the container.

The particle size and crystallization index of the powdered cellulose after the pulverization treatment can be adjusted by the supply rate of the chip-like cellulose-containing raw material to the container. Although the preferable supply rate varies depending on the volume of the container, from the viewpoint of sufficiently reducing the crystallization index, the ratio of the supply rate to the bottom area of the container (supply rate / bottom area of the container 1) is 40 kg / (min · m ² ). Or less, more preferably 30 kg / (min · m ² ) or less, and still more preferably 20 kg / (min · m ² ) or less. From the viewpoint of maintaining the throughput, the ratio of the supply rate to the bottom area of the container is preferably 0.5 kg / (min · m ² ) or more, and more preferably 1 kg / (min · m ² ) or more. It is preferably 3 kg / (min · m ² ) or more.

  The powdered cellulose produced by the production method of the present invention preferably has a median diameter reduced to 1 μm or more and 200 μm or less. The required median diameter depends on the cellulose-containing raw material used, but when the median diameter of the powdered cellulose after the pulverization treatment is 200 μm or less, the handling property is improved, the specific surface area is increased, and various chemical reactivities are obtained. improves. The median diameter of the powdered cellulose can be determined by the measurement method shown in the examples.

The powdered cellulose produced by the production method of the present invention preferably has a cellulose I-type crystallization index calculated from the above formula (1) of the contained cellulose of 50% or less.
The crystallization index is also related to the physical and chemical properties of cellulose, and the larger the value, the higher the crystallinity of cellulose and the less non-crystalline parts, so the hardness, density, etc. increase, but elongation, flexibility, Solubility and chemical reactivity in water and solvent decrease.
If the type I crystallization index of cellulose is 50% or less, the chemical reactivity of cellulose is high. From this viewpoint, the type I crystallization index of the powdered cellulose produced by the production method of the present invention is more preferably 45% or less, still more preferably 40% or less, and even more preferably 35% or less.

In relation to the above-described embodiment, the present invention discloses a method for producing powdered cellulose and a vibration grinder.
<1>
A method for producing powdered cellulose in which chip-shaped cellulose-containing raw material is pulverized using a vibration pulverizer, the vibration pulverizer having a raw material inlet and a discharge port, and having a cylindrical space inside, A container that is arranged so that the central axis of the cylindrical space is substantially horizontal, and is held so as to vibrate in an in-plane direction substantially perpendicular to the central axis, and a plurality of containers in the central axis direction inside the container, A plurality of cylindrical media, the cylindrical media are composed of two types of cylindrical media A and cylindrical media B, and satisfy the following conditions (1) to (4), Production of powdered cellulose comprising a step of introducing the cellulose-containing raw material into the container of a vibration pulverizer from the raw material inlet, pulverizing the container by vibration, and discharging the obtained powdered cellulose from the outlet Method.
(1) The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container.
(2) a cylindrical medium B, it 70mm or more in length in the central axial direction when the 110mm or less, the opening area 25 cm ² or more on the outer peripheral side surface, has at least one 250 cm ² or less of the opening, and the opening The ratio of the sum of the opening areas to the total area of the outer peripheral side surface including the portion is 10% or more and 50% or less.
(3) The cylindrical medium B is disposed so that the central axis thereof is substantially parallel to the central axis of the columnar space inside the container, and at least one cylindrical medium B satisfies the following formula: Placed in.
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance parallel to the central axis (4) The average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less.
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)
<2>
The method for producing powdered cellulose according to the above <1>, wherein the vibration pulverizer includes a raw material inlet at an upper part of the container, preferably at an upper part of one end of the container.
<3>
The vibration pulverizer has two containers at the top and bottom, and at least the upper container and the cylindrical medium disposed in the container satisfy the above conditions (1) to (4), <1> or < The method for producing powdered cellulose according to 2>.
<4>
The length in the central axis direction of the cylindrical medium A is preferably 5 mm or more, more preferably 10 mm or more, preferably 70 mm or less, more preferably 50 mm or less, any one of the above items <1> to <3> The manufacturing method of the powdered cellulose as described in any one of.
<5>
The length in the central axis direction of the cylindrical medium B is preferably 75 mm or more, more preferably 80 mm or more, preferably 100 mm or less, more preferably 95 mm or less, any one of the above items <1> to <4> The manufacturing method of the powdered cellulose as described in any one of.

<6>
Opening area per one of the openings 21 of the cylindrical media B is preferably 30 cm ² or more, more preferably 50 cm ² or more, more preferably 70cm ² or more, preferably 230 cm ² or less, more preferably 200 cm ² The manufacturing method of the powdered cellulose in any one of said <1>-<5> which is the following.
<7>
The ratio of the sum of the opening area to the total area of the outer peripheral side surface including the opening of the cylindrical medium B is preferably 20% or more, more preferably 30% or more, preferably 45% or less, more preferably The manufacturing method of the powdered cellulose in any one of said <1>-<6> which is 40% or less.
<8>
The method for producing powdered cellulose according to any one of <1> to <7> above, wherein the number of openings of the cylindrical medium B is 1 or more and 5 or less, preferably 1 or more and 4 or less.
<9>
Any one of the above items <1> to <8>, wherein at least one cylindrical medium B is disposed so as to have a position of preferably 0 ≦ d1 ≦ 0.25d, more preferably 0 ≦ d1 ≦ 0.21d. The manufacturing method of the powdered cellulose as described in any one of.
<10>
At least one cylindrical medium B is preferably positioned at 0.01 ≦ d1 ≦ 0.25d, more preferably 0.1 ≦ d1 ≦ 0.25d, and even more preferably 0.1 ≦ d1 ≦ 0.21d. The manufacturing method of the powdered cellulose in any one of said <1>-<8> arrange | positioned.

<11>
At least one cylindrical medium B is preferably arranged so as to be in a position of 0 ≦ d1 ≦ 0.2d, more preferably 0 ≦ d1 ≦ 0.1d, still more preferably 0 ≦ d1 ≦ 0.05d. The manufacturing method of the powdered cellulose in any one of said <1>-<8>.
<12>
The average gap distance between the cylindrical media is preferably 0.2 mm or more, more preferably 0.3 mm or more, preferably 5.0 mm or less, more preferably 1.0 mm or less, <1> to <11> The manufacturing method of the powdered cellulose in any one of.
<13>
Ratio of the sum of the lengths in the central axis direction of the cylindrical medium to the length in the axial direction of the cylindrical space inside the container (the sum of the lengths in the central axis direction of the cylindrical medium / the cylindrical space inside the container) Is preferably 0.80 or more, more preferably 0.85 or more, still more preferably 0.90 or more, preferably 0.995 or less, more preferably 0.99 or less, The method for producing powdered cellulose according to any one of <1> to <12>, which is preferably 0.98 or less.
<14>
The ratio of the outer diameter of the cylindrical medium to the inner diameter of the container (the outer diameter of the cylindrical medium / the inner diameter of the container) is preferably more than 0.50, more preferably 0.70 or more, and even more preferably 0.80 or more. Yes, Preferably it is 0.95 or less, More preferably, it is 0.90 or less, The manufacturing method of the powdered cellulose in any one of said <1>-<13>.
<15>
The manufacturing method of the powder cellulose in any one of said <1>-<14> provided with the grinding | pulverization medium arrange | positioned so that a vibration is further possible inside a cylindrical medium.

<16>
The ratio of the inner diameter of the cylindrical medium in contact with the grinding medium to the outer diameter of the grinding medium is 2.1 or more, preferably 2.2 or more, more preferably 2.5 or more, preferably 500 or less, more preferably Is 350 or less, more preferably 100 or less, even more preferably 50 or less, and even more preferably 25 or less, The method for producing powdered cellulose according to <15> above.
<17>
The integrated value of the volume of the grinding medium is a value exceeding 25% of the space volume inside the cylindrical medium in contact with the grinding medium, preferably 30% or more, more preferably 40% or more, preferably 90% or less, preferably The manufacturing method of the powdered cellulose as described in said <15> or <16> which is 80% or less, More preferably, it is 70% or less.
<18>
<15> to <17>, wherein the grinding medium is a rod-shaped medium having an outer diameter of 3 mm or more, preferably 5 mm or more, more preferably 7 mm or more, and 60 mm or less, preferably 50 mm or less, more preferably 45 mm or less. The manufacturing method of the powdered cellulose in any one.
<19>
The ratio of the length of the rod-shaped medium to the length in the central axis direction of the cylindrical space inside the container is 0.80 or more, preferably 0.85 or more, more preferably 0.90 or more, and 0.995. The method for producing powdered cellulose according to the above <18>, which is preferably 0.99 or less, more preferably 0.98 or less.
<20>
The difference between the inner diameter of the container and the outer diameter of the cylindrical medium in contact with the inside of the container is 3 mm or more, preferably 5 mm or more, more preferably 8 mm or more, more preferably 10 mm or more, 60 mm or less, preferably 55 mm. The method for producing powdered cellulose according to any one of <1> to <19> above, more preferably 50 mm or less, and still more preferably 45 mm or less.

<21>
The ratio of the thickness of the cylindrical medium to the outer diameter of the cylindrical medium is 0.02 or more, preferably 0.03 or more, more preferably 0.05 or more, and 0.7 or less, preferably 0.6 or less. More preferably, it is 0.5 or less, The manufacturing method of the powdered cellulose in any one of said <1>-<20>.
<22>
The cellulose content in the remaining component obtained by subtracting water from the cellulose-containing raw material of the chip-like cellulose-containing raw material is 20% by mass or more, preferably 40% by mass or more, more preferably 60% by mass or more, and still more preferably 70%. The cellulose I type crystallization index represented by the following calculation formula (1) is more than 60%, preferably 70% or more, more preferably 75% or more. The manufacturing method of the powder cellulose in any one of said <1>-<21> which is a cellulose containing raw material.
Cellulose type I crystallization index (%) = [(I _22.6 −I _18.5 ) / I _22.6 ] × 100 (1)
[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 °). Indicates. ]
<23>
The cellulose I-type crystallization index represented by the calculation formula (1) of the powdered cellulose obtained by pulverizing the chip-like cellulose-containing raw material is 50% or less, preferably 45% or less, more preferably 40% or less, The method for producing powdered cellulose according to any one of <1> to <22>, preferably 35% or less.
<24>
The water content of the chip-like cellulose-containing raw material is 0.2% by mass or more, preferably 0.3% by mass or more, more preferably 0.4% by mass or more, and 9% by mass or less, preferably 4% by mass or less. More preferably, it is 3 mass% or less, More preferably, it is 2 mass% or less, More preferably, it is 1 mass% or less, The manufacturing method of the powder cellulose in any one of said <1>-<23>.
<25>
It has a raw material inlet and outlet, has a cylindrical space inside, and is arranged so that the central axis of the cylindrical space is substantially horizontal, and vibrates in an in-plane direction substantially perpendicular to the central axis. A plurality of cylindrical media arranged in a manner capable of vibrating in the direction of the central axis inside the container, and the plurality of cylindrical media include two types of cylindrical media A and a cylindrical shape. A vibration pulverizer comprising the medium B and satisfying the above conditions (1) to (4).

<26>
The vibration pulverizer according to the above <25>, wherein the opening of the cylindrical medium B is located 10 mm or more, preferably 15 mm or more inward from the end in the central axis direction of the cylindrical medium B.

  The water content of the chip-shaped cellulose-containing raw material used in the examples and the pulverized powdered cellulose, the type I crystallization index of cellulose, the α-cellulose content, and the median diameter of the pulverized powdered cellulose, the apparent The specific gravity (hardening) was measured by the method described below.

(1) Measurement of moisture content The moisture content was measured at 120 ° C using an infrared moisture meter ("MOC-120H" manufactured by Shimadzu Corporation), and the weight change rate for 30 seconds was 0.05% or less. The end point of the measurement was taken as the end point.

(2) Calculation of crystallization index The I-type crystallization index of cellulose is obtained by using an X-ray diffractometer ["MiniFlex II" manufactured by Rigaku Corporation] to calculate the X-ray diffraction intensity of a chip-like cellulose-containing raw material or powdered cellulose. The measurement was performed under the following conditions and was calculated based on the calculation formula (1).
Measurement conditions were as follows: X-ray source: Cu / Kα-radiation, tube voltage: 30 kV, tube current: 15 mA, measurement range: diffraction angle 2θ = 5-35 °, and X-ray scan speed of 40 ° / min. The measurement sample was prepared by compressing a pellet having an area of 320 mm ² × thickness of 1 mm.

(3) Measurement of α-cellulose content α-cellulose content in the chip-like cellulose-containing raw material is 95-96 pages of the Wood Science Society of Japan, Wood Science Experiment Manual (2000, published by Buneidou Publishing Co., Ltd.). It measured based on the method of description.
First, 10 to 20 g of the raw material was weighed, placed in a Soxhlet extractor, about 150 mL of a mixed solvent having a volume ratio of ethanol and 1,2-dichloroethane of 1: 2 was added, and the mixture was boiled and refluxed for 6 hours. The sample after extraction was dried with a vacuum dryer at 60 ° C. for 4 hours to obtain a degreased sample. Take 2.5 g of the obtained defatted sample in a 300 mL Erlenmeyer flask, add about 150 mL of distilled water, 1.0 g of sodium chlorite, and 0.2 mL of acetic acid, cap the Erlenmeyer flask loosely, The contents were heated for 1 hour while occasionally shaking the contents on a hot water bath. Thereafter, 1.0 g of sodium chlorite and 0.2 mL of acetic acid were added while maintaining the temperature, and the mixture was heated on a hot water bath at 70 to 80 ° C. for 1 hour. Thereafter, the same operation as described above in which sodium chlorite and acetic acid were added and heated was repeated twice. The white contents were filtered with suction through a 1G-3 glass filter, washed with cold water and acetone, dried in a vacuum at 105 ° C. for 6 hours, and allowed to cool in a desiccator. After standing to cool, the residue on the filter was used as a holocellulose sample. The amount of holocellulose was determined as the increased weight of the filter before and after filtration, and the amount of holocellulose B (mass%) in the raw material was determined by the following formula.
B = filter weight increase / 2.5 g × 100
Take 1.0 g of the holocellulose sample in a 300 mL beaker, add 25 mL of 17.5% aqueous sodium hydroxide solution, cover the beaker with a watch glass, leave it in a constant temperature bath at 20 ° C. for 3 minutes, and then use a glass rod for 5 minutes. The sample was lightly crushed to a swollen state. The beaker was covered again with a watch glass and allowed to stand at 20 ° C., and 30 minutes after adding the aqueous sodium hydroxide solution to the sample, 25 mL of distilled water was added and stirred exactly for 1 minute. Subsequently, after leaving it for 5 minutes, it was suction-filtered with a 1G-3 glass filter, and washed quickly with 20 ° C. water until the filtrate became neutral. Further, 40 mL of 10% acetic acid is poured into the filtered contents, suction filtered to remove the liquid as much as possible, washed with 1 L of boiling water, dried in a vacuum at 105 ° C. for 6 hours, and released in a desiccator. Chilled. After standing to cool, the residue on the filter was used as an α-cellulose sample. The α-cellulose amount was determined as an increased weight of the filter before and after filtration, and the α-cellulose amount C (mass%) in holocellulose was further determined by the following formula.
C = filter increase weight / 1.0 g × 100
Next, the obtained α-cellulose sample was incinerated at 575 ° C. for 12 hours. Ash weight D (mass%) was calculated | required by the following formula | equation by weighing the weight before ashing and after ashing.
D = weight after ashing / weight before ashing × 100
From the above results, α-cellulose content E (% by mass) in the raw material from which ash was subtracted was determined by the following equation.
E = B × C ÷ 100 × (1−D ÷ 100)

(4) Measurement of median diameter The median diameter of the powdered cellulose after the pulverization treatment was measured using a laser diffraction scattering method particle size distribution measuring apparatus ["LS13 320" manufactured by Beckman Coulter, Inc.]. As the measurement conditions, pure water was used as a dispersion medium at the time of measurement, and the volume-based median diameter was measured.

(5) Measurement of apparent specific gravity (hardening) The apparent specific gravity (hardening) was measured using a powder tester (manufactured by Hosokawa Micron Corporation). An attached cap was added to the upper part of the specified container (capacity 100 mL) so that the capacity became about 200 mL. Using a scoop, the cellulose-containing raw material in the form of chips was gently put into the container, and the container was filled with the raw material. Using the tapping function of the powder tester, tapping was performed 180 times for 180 seconds. After the tapping, the cap was gently removed, the excess sample on the 100 mL container was scraped off, and the apparent specific gravity (hardened) was calculated by measuring the sample weight in the 100 mL container.

Example 1
[Cutting]
A sheet-like wood pulp (“HV +” manufactured by Tenbeck, 800 mm × 600 mm × 1.0 mm, crystallization index 80%, α-cellulose content 96 mass%, water content 8.0 mass%), which is a cellulose-containing raw material, The sheet pelletizer (“SG (E) -220” manufactured by Horai Co., Ltd.), which is a cutter, was applied to a rectangular parallelepiped having a size of about 3 mm × 1.5 mm × 1.0 mm.

[Drying treatment]
The chip-shaped cellulose-containing raw material obtained by the cutting treatment was dried using a biaxial horizontal stirring dryer (manufactured by Nara Machinery Co., Ltd., biaxial paddle dryer “NPD-1.6W (1/2)”). . The drying temperature was 140 ° C., 8 kg of the raw material was previously charged, and dried by batch treatment for 60 minutes under atmospheric pressure, so that the water content of the raw material was 0.8% by mass. Thereafter, the apparatus was tilted by 2 °, and the raw material was dried by continuous treatment. At this time, the feed rate of the raw material was 18 kg / h. The water content of the dried raw material obtained by continuous treatment was also 0.8% by mass. The obtained raw material after the drying treatment was stored in an aluminum bag until just before the pulverization treatment in order to prevent moisture absorption during storage. The cellulose type I crystallization index after the drying treatment calculated from the X-ray diffraction intensity was 81%.

[Crushing treatment]
Continuous vibration mill having two containers of the same shape at the top and bottom ("YAMT-50" manufactured by Eurus Techno Co., Ltd., inner diameter of 210 mm, axial length of cylindrical space inside the container, 820 mm, container capacity A stainless steel lining with a thickness of 6 mm was inserted into the 28.4 L container, and a cylindrical medium was placed inside the container for pulverization. In the upper stage, one stainless steel cylindrical medium A having an outer diameter of 182 mm, an inner diameter of 152 mm, and an axial length of 25.5 mm, an outer diameter of 182 mm, an inner diameter of 152 mm, a shaft from the raw material inlet side provided in the upper part of the container Cylindrical medium having a length of 90 mm in the direction and 15 mm inside from both ends in the central axis direction, and equally four rectangular openings of 60 mm in the axial direction and 80 mm in the circumferential direction on the outer peripheral side surface 27 stainless steel cylindrical media A having one B, an outer diameter of 182 mm, an inner diameter of 152 mm, and an axial length of 25.5 mm, each in a direction in which the axial direction of the cylindrical media is parallel to the axial direction of the container Arranged. When the longest distance parallel to the central axis from the center of the container raw material inlet to the end of the cylindrical space inside the container in the direction of the central axis is d, the cylindrical medium B is from the center of the raw material inlet of the container. The distance d1 parallel to the central axis to the center of the opening of the cylindrical medium B is arranged at a position of 0.00067d. At this time, the opening area ratio of the cylindrical medium B was 37.3%, and the average gap distance between the upper cylindrical media was 0.53 mm.
In the lower stage of the continuous vibration mill, 31 stainless steel cylindrical media A each having an outer diameter of 182 mm, an inner diameter of 152 mm, and an axial length of 25.5 mm, and the axial direction of the cylindrical media A is parallel to the axial direction of the container. Arranged in the direction to become.
Chip-like cellulose-containing raw material (apparent specific gravity (hardened) 0.18 g / mL) obtained by the drying process is fed into the container from the raw material inlet at the upper stage of the vibration mill at a supply rate of 8.3 kg / (min · m ² ). Continuously supplied, the container is vibrated under the conditions of an amplitude of 8 mm and a vibration frequency of 20 Hz to pulverize the chip-like cellulose-containing raw material, and the powdery cellulose is continuously discharged from the lower outlet to obtain powdered cellulose. It was. The results are shown in Table 1.

Example 2
In Example 1, the cylindrical medium B has an outer diameter of 182 mm, an inner diameter of 152 mm, and an axial length of 90 mm. The axial length is 60 mm × the circumferential length of 320 mm, 15 mm inside from both ends in the central axis direction. The powdered cellulose was produced in the same manner as in Example 1 except that the cylindrical opening B having one rectangular opening was provided on the outer peripheral side surface. The results are shown in Table 1.

Examples 3-4
Powdered cellulose was produced in the same manner as in Example 1 except that the arrangement of the cylindrical medium B was changed as shown in Table 1. The results are shown in Table 1.

Example 5
A cylindrical cylindrical medium made of stainless steel having an outer diameter of 30 mm and a length of 800 mm as a grinding medium (the length of the rod-shaped medium / the cylindrical shape inside the container) inside the cylindrical medium arranged in the upper and lower stages of the continuous vibration mill The length in the axial direction of the space is 0.976) in each case (the integrated value of the volume of the rod-shaped medium with respect to the space volume inside the cylindrical medium = 62.3%). Powdered cellulose was produced by the method described above. The results are shown in Table 1.

Comparative Example 1
The same method as in Example 1 except that the cylindrical medium disposed in the upper stage of the continuous vibration mill was replaced with 31 stainless steel cylindrical mediums A having an outer diameter of 182 mm, an inner diameter of 152 mm, and an axial length of 25.5 mm. In this way, powdered cellulose was produced. The results are shown in Table 1.

Comparative Example 2
In Example 1, the cylindrical medium B has an outer diameter of 182 mm, an inner diameter of 152 mm, an axial length of 90 mm, and an axial length of 60 mm × circumferential length of 15 mm inside 15 mm from both ends in the central axis direction. The powdered cellulose was produced in the same manner as in Example 1 except that the cylindrical opening B having four rectangular openings was provided on the outer peripheral side surface. The results are shown in Table 1.

Comparative Example 3
Powdered cellulose was produced in the same manner as in Example 1 except that the arrangement of the cylindrical medium B was changed as shown in Table 1. The results are shown in Table 1.

  According to the vibration pulverizer of the present invention and the method for producing powdered cellulose using the vibration pulverizer, the chip-shaped cellulose-containing raw material can be introduced into the vibration pulverizer without clogging. Therefore, even if the supply rate of the chip-like cellulose-containing raw material is high, powdered cellulose having a reduced particle size can be efficiently produced without causing clogging. Therefore, the method for producing powdered cellulose of the present invention is excellent in productivity and useful as an industrial production method.

DESCRIPTION OF SYMBOLS 1 Container 11 Raw material inlet 12 Outlet 13 Cover part 2A Cylindrical medium A
2B Cylindrical medium B
21 Opening 21B of cylindrical medium B Center line passing through the center of the opening of cylindrical medium B and perpendicular to the axial direction 3 Grinding medium (columnar rod-shaped medium)
100 Vibration crusher

Claims (11)

A method for producing powdered cellulose in which chip-shaped cellulose-containing raw materials are pulverized using a vibration pulverizer,
The vibration pulverizer includes a raw material inlet and an outlet, has a cylindrical space inside, and is arranged so that a central axis of the cylindrical space is substantially horizontal, and is substantially perpendicular to the central axis. A container held so as to vibrate in an in-plane direction,
A plurality of cylindrical media arranged in the container so as to be capable of vibrating in the central axis direction;
The plurality of cylindrical media are composed of two types of cylindrical media A and cylindrical media B, and satisfy the following conditions (1) to (4):
Introducing the cellulose-containing raw material into the container of the vibration pulverizer from the raw material inlet, pulverizing the container by vibrating, and discharging the obtained powdered cellulose from the outlet, Production method.
(1) The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container.
(2) a cylindrical medium B, it 70mm or more in length in the central axial direction when the 110mm or less, the opening area 25 cm ² or more on the outer peripheral side surface, has at least one 250 cm ² or less of the opening, and the opening The ratio of the sum of the opening areas to the total area of the outer peripheral side surface including the portion is 10% or more and 50% or less.
(3) The cylindrical medium B is disposed so that the central axis thereof is substantially parallel to the central axis of the columnar space inside the container, and at least one cylindrical medium B satisfies the following formula: Placed in.
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance parallel to the central axis (4) The average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less.
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)   The manufacturing method of the powdered cellulose of Claim 1 with which a vibration crusher equips a container upper part with a raw material inlet.   The method for producing powdered cellulose according to claim 1 or 2, wherein the number of openings of the cylindrical medium B is 1 or more and 5 or less.   The manufacturing method of the powdered cellulose of any one of Claims 1-3 provided with the grinding | pulverization medium arrange | positioned so that a vibration is further possible inside a cylindrical medium.   The method for producing powdered cellulose according to claim 4, wherein the grinding medium is a rod-shaped medium having an outer diameter of 3 mm or more and 60 mm or less.   The method for producing powdered cellulose according to any one of claims 1 to 5, wherein a difference between the inner diameter of the container and the outer diameter of the cylindrical medium in contact with the inside of the container is 3 mm or more and 60 mm or less.   The method for producing powdered cellulose according to any one of claims 1 to 6, wherein the ratio of the thickness of the cylindrical medium to the outer diameter of the cylindrical medium is 0.02 or more and 0.7 or less. The cellulose content in the chip-shaped cellulose-containing raw material is 20% by mass or more in the remaining components obtained by subtracting water from the cellulose-containing raw material, and the cellulose I-type crystallization index represented by the following formula (1) is 60 The manufacturing method of the powdered cellulose of any one of Claims 1-7 which is a cellulose containing raw material exceeding%.
Cellulose type I crystallization index (%) = [(I _22.6 −I _18.5 ) / I _22.6 ] × 100 (1)
[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 °). Indicates. ]   The cellulose I type crystallization index | exponent shown by the said Formula (1) of the powdered cellulose obtained by grind | pulverizing a chip-shaped cellulose containing raw material is 50% or less, The any one of Claims 1-8. Of manufacturing powdered cellulose. It has a raw material inlet and outlet, has a cylindrical space inside, and is arranged so that the central axis of the cylindrical space is substantially horizontal, and vibrates in an in-plane direction substantially perpendicular to the central axis. A container that can be held, and a cylindrical medium that is arranged in the container so as to be able to vibrate in the direction of the central axis.
The plurality of cylindrical media are vibration pulverizers comprising two types of cylindrical media A and cylindrical media B and satisfying the following conditions (1) to (4).
(1) The cylindrical medium A has a length in the central axis direction of 3 mm or more and 100 mm or less, and is arranged so that the central axis is substantially parallel to the central axis of the cylindrical space inside the container.
(2) a cylindrical medium B, it 70mm or more in length in the central axial direction when the 110mm or less, the opening area 25 cm ² or more on the outer peripheral side surface, has at least one 250 cm ² or less of the opening, and the opening The ratio of the sum of the opening areas to the total area of the outer peripheral side surface including the portion is 10% or more and 50% or less.
(3) The cylindrical medium B is disposed so that the central axis thereof is substantially parallel to the central axis of the columnar space inside the container, and at least one cylindrical medium B satisfies the following formula: Placed in.
0 ≦ d1 ≦ 0.3d
d1: Distance parallel to the central axis from the center of the raw material inlet of the container to the center of the opening of the cylindrical medium B d: End of the cylindrical space in the central axis direction from the center of the raw material inlet of the container The longest distance parallel to the central axis (4) The average gap distance between the cylindrical media calculated by the following formula is 0.1 mm or more and 30 mm or less.
Average gap distance = (length of container in the central axis direction−total length of cylindrical medium in the central axis direction) / (number of cylindrical media + 1)   The vibration pulverizer according to claim 10, wherein the opening of the cylindrical medium B is located at least 10 mm inside the end of the cylindrical medium B in the central axis direction.

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