JP2005207854A - Method for testing filling strength of sample particles - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a testing method capable of measuring the filling strength of catalyst particles (2) as their deformability and the dispersibility of the particle sizes. <P>SOLUTION: A particle-filling part (6) is constituted of a base (3a), a first side surface (41a), a second side surface (42a), a third side surface (43a), and a pressing surface (5a) movable along these surfaces, and has an upward opened structure, and is filled with test particles 2 to form a particle-filled bed (20) and the pressing surface (5a) is moved at a constant moving speed (V) to compress the particle-filled bed (20) to calculate yield pressure (τ). A plurality of yield pressures (τ) are measured by changing the moving speed (V), and the displaceability of the test particles (2) is calculated from the coefficient (m), satisfying the formula (I): log(τ)=m×log(V)+log(a); and the dispersibility of the particle sizes of the test particles is calculated from the coefficient (a). A testing machine (1) is equipped with a moving means (7) for moving the pressing surface (5a), and a pressure measuring means (8) for measuring the pressure applied to the particle filled bed (20). <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

The present invention relates to a method for testing the packing strength of sample particles.

As shown in FIG. 5, the fixed bed reactor (A) in which the catalyst particles (2) are filled in the reaction vessel (B) and fixed as the catalyst particle packed bed (20) is, for example, a hydrocarbon gas, It is widely used as a reforming reaction apparatus for producing a product gas (D) containing hydrogen or the like from a raw material gas (C) such as alcohol gas. In such a fixed bed reactor (A), the raw material gas (C) is converted into the product gas (D) while passing through the catalyst particle packed bed (20).

The reactor (A) is in a state of being heated to a high temperature of 300 ° C. to 700 ° C. from the outside during operation, for example. On the other hand, after the operation is stopped, it is cooled to room temperature, for example, about 20 ° C. or less. It becomes a state. When the operation and the stop are repeated, the catalyst particles (2) and the reaction vessel (7) are repeatedly expanded and contracted, and stress is applied to the catalyst particle packed bed (20). If stress is applied to the catalyst particle packed bed (20), the catalyst particles (2) may be broken and pulverized. The finely divided catalyst particles (2) prevent passage of the raw material gas (C). For this reason, the catalyst particles (2) are required to have a high packing strength and are not easily destroyed even when stress is applied in the packed state.

Conventionally, as a method for testing the packing strength of sample particles (2), as shown in FIG. 1, a horizontal bottom surface (3a), a planar first side surface (41a) and a second side surface (42a) are used. And a packed particle layer (6) filled with a sample particle (2) in a particle packed portion (6) having a flat third side surface (33a) and a pressurizing surface (5a). (20) is formed, the pressure surface (5a) is moved to a predetermined position, the particle packed bed (20) is compressed, and the proportion of the sample particles (2) is determined from the ratio of the broken particles (2). A method for determining the filling strength has been known [Patent Document 1: Japanese Patent Laid-Open No. 5-126706].

Japanese Patent Laid-Open No. 5-126706

However, according to the study by the present inventor, it has been found that, even in the case of such a conventional test method, even particles having a high packing strength may not always show a sufficient strength in an actual reactor.

Therefore, as a result of intensive studies to develop a test method for filling strength that reflects the strength in the actual reaction vessel, the present inventor has found that the expansion and contraction accompanying the start and stop of operation are uniform in the actual reaction vessel. However, even if the catalyst particles show a high or high filling strength against a slow expansion / contraction, the catalyst has a high filling strength against a sudden expansion / contraction. According to the test method for determining the yield pressure of the particle packed bed by moving the pressure surface at a constant moving speed and determining the yield pressure of the particle packed bed, a plurality of yield pressures are changed by changing the moving speed. By measuring, it was found that the filling strength against the gentle expansion / contraction can be obtained, and at the same time, the filling strength against the rapid expansion / contraction can be obtained.

That is, the present invention comprises a horizontal bottom surface (3a),
The first side surface (41a) and the second side surface (42a) which are fixed upright from the bottom surface (3a) and face each other in parallel,
A third side surface (43a) that is fixed upright from the bottom surface (3a) and orthogonal to the first side surface (41a) and the second side surface (42a);
It is perpendicular to the bottom surface (3a), the first side surface (41a) and the second side surface (42a), and is movable along the bottom surface (3a), the first side surface (41a) and the second side surface (42a). The particle filling section (6) is configured with a pressing surface (5a) and the upper part is open,
Fill the sample particles (2) to form a particle packed bed (20),
The pressurized surface (5a) is moved along the bottom surface (3a), the first side surface (41a) and the second side surface (42a) at a constant moving speed (V) to compress the particle packed bed (20). The yield strength (τ) of the particle packed bed (20) is obtained, and a method for testing the packing strength of the sample particles (2) is provided.

1 to 3 show a test apparatus (1) for testing the filling strength of sample particles (2) by the test method of the present invention. This test apparatus (1) includes a particle packing section (6) for forming a particle packing layer (20). As described above, the particle packed portion (6) has a horizontal bottom surface (3a), and
The first side surface (41a) and the second side surface (42a) which are fixed upright from the bottom surface (3a) and face each other in parallel,
A third side surface (43a) that is fixed upright from the bottom surface (3a) and orthogonal to the first side surface (41a) and the second side surface (42a);
It is perpendicular to the bottom surface (3a), the first side surface (41a) and the second side surface (42a), and is movable along the bottom surface (3a), the first side surface (41a) and the second side surface (42a). And a pressing surface (5a). The test apparatus (1) also includes a moving means (7) for moving the pressure surface (5a) along the bottom surface (3a), the first side surface (31a), and the second side surface (32a) at a constant moving speed (V). )When,
Pressure measuring means (8) for measuring the pressure applied to the particle packed bed (20) formed in the particle packed section (6) from the pressure surface (5a) when moved by the moving means (7). . Then, the moving means (7) moves the pressure surface (5a) along the bottom surface (3a), the first side surface (41a) and the second side surface (42a) at a constant moving speed (V). While compressing the particle packed bed (20), the pressure applied to the particle packed bed (20) from the pressure surface (5a) can be measured by the pressure measuring means (8).

According to the test method of the present invention, not only the packing strength of the catalyst particles against a gradual increase in stress, but also the packing strength against an abrupt increase in stress can be obtained.

Hereinafter, the test method of the present invention will be described with reference to FIGS.
In order to obtain the yield pressure (τ) by the test method of the present invention, first, the particle packed portion (6) is filled with the sample particles (2) to form the particle packed layer (20). 1 to 3 show a state in which a particle packed layer (20) is formed in a particle packed portion (6), FIG. 1 is a perspective view, FIG. 2 is a side sectional view, and FIG. 3 is a longitudinal sectional view. It is.

The particle packing section (6) includes a horizontal planar bottom surface (3a), a planar first side surface (41a) and a second side surface (42a), a third side surface (43a), and a pressure surface (5a). It is configured.

Although the bottom surface (3a) may be strictly a horizontal plane, in practice, it may be generally a horizontal plane. The bottom surface (3a) is constituted by, for example, a bottom plate (3).

The first side surface (41a) and the second side surface (42a) are planar and may be strictly planar, but practically may be substantially planar. The first side surface (41a) and the second side surface (42a) are surfaces upstanding from the bottom surface (3a), and are thus orthogonal to the bottom surface (3a) when viewed from the side. The first side surface (41a) and the second side surface (42a) may be strictly upright from the bottom surface (3a), but in practice, they may be generally upright. The first side surface (41a) and the second side surface (42a) are fixed to the bottom surface (3a). The first side surface (41a) and the second side surface (42a) are parallel to each other. Here, the first side surface (41a) and the second side surface (42a) may be strictly parallel, but may be practically substantially parallel. Further, the first side surface (41a) and the second side surface (42a) are opposed to each other to form the particle packing portion (6). The first side surface (41) and the second side surface (42) are constituted by a first side plate (41) and a second side plate (42), respectively.

Since the third side surface (43a) is a surface upright from the bottom surface (3a), it is orthogonal to the bottom surface (3a) when viewed from the side. The third side surface (43a) may be strictly upright from the bottom surface (3a), but in practice, it may be generally upright. The third side surface (43a) is fixed to the bottom surface (3a). The third side surface (43a) is also orthogonal to the first side surface (41a) and the second side surface (42a) when viewed from above. Here, the third side surface (43a) may be strictly orthogonal, but in practice, it may be substantially orthogonal. The third side surface (43a) is preferably planar. The third side surface (43a) is constituted by a third side plate (43).

The bottom plate (3), the first side plate (41), the second side plate (42), and the third side plate (43) may be configured integrally or assembled as separate bodies. It may be configured.

The pressing surface (5a) is orthogonal to the bottom surface (3a) when viewed from the side. Further, the first side surface (41a) and the second side surface (42a) are orthogonal to each other when viewed from above. The pressurizing surface (5a) may be strictly orthogonal to these surfaces (3a, 41a, 42a, 43a), but may be practically approximately orthogonal. The pressing surface (5a) is configured to be movable along the bottom surface (3a), the first side surface (41a), and the second side surface (42a). The pressure surface (5a) is configured as one surface of the pressure plate (5).

On the bottom surface (3a), the particle packing portion (6) is surrounded on its side by the first side surface (41a), the second side surface (42a), the third side surface (43a), and the pressure surface (5a). . The upper part is open.

The size of the particle filling portion (6) is, for example, about 2 cm to 15 cm on one side and about 5 cm to 7 cm in height on the bottom surface (3a).

Examples of the sample particles (2) filled in the particle filling section (6) include catalyst particles used for gas phase catalytic oxidation. Moreover, catalyst carrier particles are also included. The catalyst carrier particles are raw materials used to produce catalyst particles by supporting a catalyst component on the surface. The particle diameter of the sample particles (2) is usually about 0.5 mm to 10 mm. Since the spherical sample particles (2) generally have high displaceability in general, the test method of the present invention is suitable when the sample particles (2) are spherical.

In the test method of the present invention, after the particle packed bed (20) is formed, the pressed surface (5a) is moved to compress the particle packed bed (20). In the apparatus (1) shown in FIG. 1, as shown in FIG. 2, a moving means (7) is provided behind the pressure surface (5a), and the pressure surface (5a) is moved by the moving means (7). Let Examples of the moving means (7) include a crank mechanism in which the rotational output from the electric motor (M) is decelerated by the speed reducer (G) and the pressure surface (5a) is linearly driven by the crank (C). Moreover, the piston etc. which drive linearly with compressed air etc. are mentioned. The moving speed (V) for moving the pressing surface (5a) is usually selected from the range of about 1 mm / min to 1000 mm / min. The moving speed (V) is constant and may be strictly constant, but it may be practically substantially constant. The pressure surface (5a) moves along the bottom surface (3a), the first side surface (41a), and the second side surface (42a).

In the test method of the present invention, the yield pressure (τ) of the particle packed bed is obtained while compressing the particle packed bed (20). The yield pressure (τ) can be obtained by measuring the pressure applied to the particle packed bed (20) from the pressing surface (5a) while compressing the particle packed bed (20).

FIG. 4 schematically shows an example in which the pressure (P) applied from the pressure surface (5a) to the particle packed bed (20) when the pressure surface (5a) is moved is measured. The horizontal axis indicates the position (L) of the pressure surface, and the vertical axis indicates the pressure (P). As the pressure measuring means (8) for measuring the pressure (P), for example, when the crank mechanism described above is used as the moving means (7), a piezoelectric element for measuring the force applied to the crank (C) can be mentioned. . The measuring means may be configured to calculate the pressure (P) by measuring the distortion of the crank using a strain gauge or the like. Further, it may be configured to calculate from the rotation speed, current value, voltage value, etc. of the electric motor (M). When a piston or the like is used as the moving means, measurement may be performed from the supply amount of compressed air supplied to the piston, the pressure in the piston, or the like.

In FIG. 4, when the movement of the pressure surface (5a) is started (L = 0), the particle packed bed (20) is not yet compressed and the pressure (P) is zero. While moving to a position where pressing surface (5a) is represented by L = L ₁ is gradually compressed particle packing layer (20), the pressure required to move the pressure surface (5a) (P) gradually increases. Moreover, continued movement of the pressure face (5a), so when it comes to L> L _1, the pressure required to move the pressure surface (5a) (P) is generally exhibits a constant yield pressure, yield this pressure What is necessary is just to read as a pressure (tau).

Thus, the yield pressure (τ) of the particle packed bed (20) when the pressing surface (5a) is moved at a constant speed (V) can be obtained.

According to the method of the present invention, a plurality of yield pressures (τ) are measured by changing the moving speed (V), and the equation (I) is calculated from the moving speed (V) and the measured yield pressure (τ).
log (τ) = m × log (V) + log (a) (I)
Can be obtained. The coefficient a is an index indicating the packing strength of the sample particles (2) when the stress applied to the sample packing layer (20) is gently increased. The smaller the coefficient a, the easier the sample particles (2) to break when the stress increases gently, and the larger the coefficient a, the more difficult the sample particles (2) break when the stress increases gently. .

Similarly, the coefficient m satisfying the above formula (I) can be obtained from the moving speed (V) and the measured yield pressure (τ). The coefficient m is an index indicating the packing strength of the sample particles (2) when the stress rapidly increases compared to when the stress gradually increases. If the coefficient m is small, even if the coefficient a is large and the sample particles (2) are not easily broken when the stress rises gently, they tend to break when the stress rises rapidly. In addition, the larger the coefficient m, the less likely the sample particles (2) that are fragile when the coefficient a is small and the stress rises slowly, are less likely to break when the stress is suddenly increased. It is in.

In order to obtain a plurality of yield pressures (τ), the same operation as described above may be performed while replacing the sample particles (2) filled in the particle packed bed (20). The yield pressure (τ) may be obtained only for the moving speed (V) at two points, but is preferably obtained for the moving speed (V) at at least three points.

Next, a coefficient m satisfying the above formula (I) is obtained from the moving speed (V) and the obtained yield pressure (τ). The coefficient m can be easily obtained by a normal method such as a regression calculation method.

EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by this Example.

Example 1
As shown in FIG. 1 to FIG. 3, it is composed of a bottom surface (3a), a first side surface (41a), a second side surface (42a), a third side surface (43), and a pressure surface (5a). The particle packed part (6) having a height of 7 cm is filled with commercially available activated alumina spherical particles (manufactured by Sumitomo Chemical Co., Ltd., “KHD-12”, outer diameter is about 1 mm to 2 mm). 20) was formed. Next, the pressure surface (5a) was moved at a speed (V) of 3.3 m / min. At this time, the pressure (P) applied from the pressure surface (5a) to the particle packed bed (20) was moved while being measured by a pressure measuring device (8) provided behind the pressure plate (5). The movement was performed by a linear drive mechanism (7) driven by an electric motor (not shown). FIG. 4 shows the relationship between the position of the pressing surface (5a) and the pressure (P). Table 1 shows the results of determining the yield pressure (τ) from the relationship between the pressure surface position (L) and the pressure (P). The compressive strength measured with the Kiya-type compressive strength measuring device is also shown.

After the measurement, the yield pressure (τ) was determined in the same manner as described above except that the total amount of the activated alumina spherical particles was changed and the moving speed (V) was changed to 33 m / min. Further, the yield pressure (τ) was determined in the same manner as described above except that the total amount of the activated alumina spherical particles was changed and the moving speed (V) was changed to 333 m / min. The results are shown in Table 1.

From each moving speed (V) and the obtained yield pressure (τ), coefficient m and coefficient a satisfying the expression (1) were obtained by regression calculation. The results are shown in Table 2.

Example 2 to Example 4
Instead of activated alumina spherical particles [KHD-12], activated alumina spherical particles [manufactured by Sumitomo Chemical Co., Ltd., “KHD-24”, outer diameter of about 2 mm to 4 mm] (Example 2), activated alumina spherical particles [ “KHD-46” manufactured by Sumitomo Chemical Co., Ltd., outer diameter of about 4 mm to 6 mm] (Example 3) and resin particles [acrylonitrile-styrene-butadiene resin (ABS resin), outer diameter of about 6 mm] (Example) By operating in the same manner as in Example 1 except that 4) was used, the yield pressure (τ) was determined for the moving speed (V) of 3.3 M / min, 33 m / min, and 333 m / min. The results are shown in Tables 1 and 2.

Table 1
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Spherical particle movement speed Yield stress Compressive strength
(m / min) (N / cm ² ) (N)
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Example 1 KHD-12 3.3 1.23 54.9
33 1.62
333 1.90
Example 2 KHD-24 3.3 0.74 131.8
33 0.80
333 1.03
Example 3 KHD-46 3.3 0.80 254.5
33 0.94
333 0.98
Example 4 Resin particles 3.3 0.67 330.5
33 0.78
333 0.89
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━

Table 2
━━━━━━━━━━━━━━━━━━━━━━━━━━━
Spherical particle coefficient m coefficient a
━━━━━━━━━━━━━━━━━━━━━━━━━━━
Example 1 KHD-12 0.049 1.358
Example 2 KHD-24 0.051 0.720
Example 3 KHD-46 0.026 0.838
Example 4 Resin particles 0.034 0.705
━━━━━━━━━━━━━━━━━━━━━━━━━━━

It is a perspective view for demonstrating the method to test a packed bed intensity | strength. It is a sectional side view which shows an example of the testing apparatus for testing a packed bed intensity | strength. It is a longitudinal cross-sectional view which shows an example of the testing apparatus for testing a packed bed intensity | strength. In this example, the pressure (P) applied to the particle packed bed from the pressing surface is measured, the horizontal axis indicates the position (L) of the pressing surface, and the vertical axis indicates the pressure (P). It is sectional drawing which shows an example of a fixed bed reaction apparatus typically.

Explanation of symbols

1: Packing strength test device 2: Sample particles 20: Particle packed bed
3a: Bottom 3: Bottom plate
41a: First side 41: First side plate
42a: second side 42: second side plate
43a: Third side 43: Third side plate
5a: Pressurizing surface 5: Pressurizing plate 6: Particle filling unit 7: Moving means 8: Pressure measuring means V: Moving speed of the pressing surface τ: Yield pressure of the particle packed bed L: Position of the pressing surface P: Pressure A: Fixed bed Reactor B: Reaction vessel C: Raw material gas D: Product gas

Claims (4)

A horizontal bottom surface, a planar first side surface and a second side surface which are fixed upright from the bottom surface and face each other in parallel, and a first side surface and a second side surface which are fixed upright from the bottom surface. A third side surface orthogonal to the bottom surface, the first side surface and the second side surface, and a pressure surface movable along the bottom surface, the first side surface and the second side surface. In the particle packing part of the configuration where is opened, the sample particles are packed to form a particle packed layer,
Compressing the particle packed bed by moving the pressure surface along the bottom surface, the first side surface, and the second side surface at a constant moving speed (V) to obtain a yield pressure (τ) of the particle packed layer. A method for testing the filling strength of the sample particles. A plurality of yield pressures (τ) are measured by changing the moving speed (V) of the pressing surface,
From the moving speed (V) and the measured yield pressure (τ), the formula (I)
log (τ) = m × log (V) + log (a) (I)
The test method according to claim 1, wherein a coefficient a satisfying A plurality of yield pressures (τ) are measured by changing the moving speed (V) of the pressing surface,
From the moving speed (V) and the measured yield pressure (τ), the formula (I)
log (τ) = m × log (V) + log (a) (I)
The test method according to claim 1 or 2, wherein a coefficient m satisfying the above is obtained. A horizontal bottom surface, a planar first side surface and a second side surface which are fixed upright from the bottom surface and face each other in parallel, and a first side surface and a second side surface which are fixed upright from the bottom surface. A third side surface orthogonal to the bottom surface, the first side surface and the second side surface, and a pressure surface which is movable along the bottom surface, the first side surface and the second side surface. In addition to a configuration in which the upper part is opened, a particle filling part for filling a sample particle to form a particle packed layer is provided,
A moving means for moving the pressurizing surface along the bottom surface, the first side surface and the second side surface at a constant moving speed, and a pressure for measuring a pressure applied to the particle packed layer from the pressurizing surface when the moving surface is moved by the moving means. Measuring means,
The pressing means moves the pressing surface along the bottom surface, the first side surface, and the second side surface at a constant moving speed while compressing the particle packed layer formed in the particle packing portion from the pressing surface. The apparatus for testing the filling strength of the sample particles, wherein the pressure applied to the particle packed bed can be measured by the pressure measuring means.

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