JP2963333B2 - Softening point measuring device and softening point measuring method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a softening point measuring apparatus and a softening point measuring method for measuring the softening point of a sample such as asphalt, and more particularly, to a softening point capable of measuring the softening point of a sample in a short time and easily. The present invention relates to a measuring device and a method for measuring a softening point.

[0002]

2. Description of the Related Art The softening point is the temperature of a sample such as asphalt when the sample starts to soften and hangs down to a specified distance (25.4 mm) when heated under specified conditions. Then, the measurement method is JIS K22
07. The softening point test method according to K2207 is a so-called ring and ball method, and is generally performed as follows.

In the softening point test method according to K2207, a softening point tester 70 as shown in FIG. 4 is used. In FIG. 4, reference numeral 72 denotes a heating bath in which a ring base 74 is installed. First, the openings of the two shoulder rings 76 (see FIG. 5) are filled with a molten sample, cooled and solidified, placed on the ring base 74, respectively, and further, a thermometer 78 and a ball guide 80 are provided.
(See FIG. 6) is assembled on a ring base 74 in the heating bath 72.
5 (a) is a plan view of the shoulder ring 76, FIG. 5 (b) is a partial sectional side view thereof, FIG. 6 (a) is a plan view of the ball guide 80, and FIG. It is the side view. If the softening point of the sample is below 80 ° C, use distilled water boiled and cooled to 5 ° C. If the softening point exceeds 80 ° C,
Glycerin at about 32 ° C.
Fill up to a height of 8mm. The bath temperature should be 5 ° C if the softening point is below 80 ° C, 32 ° C if it exceeds 80 ° C,
Hold for 15 minutes.

[0004] A ball 82 having a diameter of about 9 mm, which has been previously heated to the bath temperature, is placed at the center of the ball guide 80 with tweezers, and heating of the heating bath 72 is started. From 3 minutes after the start of heating, until the softening point is reached, heating is performed so that the bath temperature uniformly increases at a rate of 5 ± 0.5 ° C. per minute. The sample softens and expands, and the ball 82
The thermometer reading when the bottom plate 84 of No. 4 is touched is read, and this is defined as the softening point. More precisely, the average temperature of the two balls on the left and right is defined as the softening point. In FIG. 4, reference numeral 86 denotes a work table having a built-in heating element 88 and a temperature control device (not shown). The ring base 74 includes a bottom plate 84 and a middle plate 90 for supporting the shoulder ring 76. The middle plate 90 is provided with a through hole so that the ball 82 falls to the bottom plate 84 when the sample is softened.

[0005]

In a petroleum refining plant for producing petroleum products from crude oil or a chemical plant for producing low-flowable substances, it is often necessary to measure the softening point. For example, in the process of producing blown asphalt in an oil refinery, it is necessary to frequently measure the softening point of asphalt. With blown asphalt, heavy oil is introduced into a vacuum distillation unit and distilled, and as a result, soft straight asphalt that flows out of the bottom as a residual oil is heated, air is blown, and oxidation, polymerization, condensation, etc. It is asphalt made.

[0006] In a batch production apparatus for blown asphalt, the softening point is frequently measured in the final stage of conversion from straight asphalt to blown asphalt,
It is necessary to adjust reaction conditions and the like based on the measured softening point. In one production process of blown asphalt,
It takes about 7 to 8 hours, but in the latter half of the manufacturing process, the blown-asphaltization reaction progresses rapidly, and the softening point rises about 10 ° C in 1 hour. To manage production conditions and softening point,
It is necessary to quickly measure the softening point of the sample in the device.

However, the above-mentioned softening point test method according to JIS K2207 can measure the softening point strictly, but it takes 2 to 3 hours to measure the softening point of one sample, and it is necessary to use a blown asphalt. It was not possible to quickly measure the softening point of a sample taken from the device as the reaction proceeded. In addition, it requires a large measuring device,
In addition, every time after sample measurement, it takes human labor to clean the above-mentioned ring base, shoulder ring, thermometer, and ball guide, so it can meet the demand for easy measurement of softening point at the manufacturing site. Did not. Therefore, at the manufacturing site, blown asphalt was actually manufactured based on the experience and intuition of the operator. This made it difficult to make the quality of blown asphalt products uniform and to make the manufacturing process more efficient.

Accordingly, an object of the present invention is to provide a softening point measuring apparatus and a softening point measuring method capable of promptly measuring the softening point of a sample in response to the requirements of a manufacturing site.

[0009]

Means for Solving the Problems The present inventor has proposed JISK2
207 strictly regulates the heating rate of the heating bath and requires time for sample preparation, so it is considered extremely difficult to reduce the time required for measurement. The temperature of JISK
Correlation with the softening point measured by the method of 2207 was studied. In the softening point test method of JIS K2207, the molten sample is cooled once, and the cooled sample is reheated to measure the softening point. However, the present inventor has used blown powder to reduce the time required for sample preparation. The focus was on measuring the softening point in the process of solidification of the molten sample collected from the asphalt production equipment. Further, based on this viewpoint, the present inventor studied a softening point measuring device and a measuring method capable of obtaining a specific measurement factor which can be easily correlated with the softening point measured by the softening point test method of JIS K2207. Was completed.

In order to achieve the above object, a softening point measuring apparatus according to the present invention comprises: a rotating plate for rotating an open container containing a sample whose softening point is to be measured on a rotation center on an upper surface; A rotating device for rotating the sample, a thermometer for measuring the temperature of the sample in the container, and a rotating device that descends vertically into the container, dipped in the sample in the container, and rotates around the longitudinal axis due to adhesion with the sample. An indicator rod and a rotation indicator for measuring a rotation angle of the rotation indicator rod are provided.

The rotation indicator rod used in the present invention is constituted by a rod-shaped body, and the lower part of the rod-shaped body is immersed in a sample in a container, and rotates around its longitudinal axis due to adhesion with the sample. The rotation indicator is a device that measures the rotation angle of the rotation indicator rod, and is a known device that optically, electrically, or mechanically measures the angle.

In a preferred embodiment of the present invention, the thermometer is a rod-shaped thermometer which is rotatably hung by a hanging tool, immerses a lower portion of the thermometer in a sample in the container, and measures the temperature of the sample. And, the rotation indicator rod, which extends in a direction perpendicular to the longitudinal direction of the rod-shaped thermometer, and has an indicator for indicating the rotation angle of the rod-shaped thermometer that rotates around the longitudinal axis due to adhesion with the sample, It is characterized by being an integrally formed thermometer. In this embodiment, a rod-shaped thermometer is used as a thermometer, and the upper part thereof is used as a rotation indicator rod by hanging it with a hanging tool. Thereby, the configuration of the present invention can be simplified. The hanging tool may be a rotatable ordinary joint, for example, a universal joint, but is preferably a deformable thread such as cotton thread, cotton thread, or nylon thread. When the thermometer is hung by these yarns, the thermometer becomes vertically autonomous and can freely rotate around the longitudinal axis.

A further preferred embodiment of the present invention is characterized in that the container is a disposable paper container. This eliminates the need for cleaning the sample container, thus making the measurement even easier.

The softening point measuring method according to the present invention is characterized in that an open container containing a molten sample whose softening point is to be measured is placed on the center of rotation on a rotating plate, and a thermometer whose upper part is hung by a hanging thread has a longitudinal direction. Insert the rotating plate into the sample in the container so that it points to the center of rotation, drive the rotating plate to rotate it, and measure the rotation angle of the thermometer with the indicator that extends in the direction perpendicular to the longitudinal direction of the thermometer. Measuring the sample temperature at the time when the thermometer rotates a predetermined rotation angle, and obtaining the softening point of the sample based on the sample measurement temperature in accordance with the correlation between the previously determined softening point and the sample measurement temperature. And

The predetermined rotation angle is the number of rotations of the rotary table,
Depending on the properties of the sample, the rotation speed of the rotary table is 3
In the range of ~ 12 rpm, preferably from 90 ° to 360 °
Range, more preferably in the range of 150 ° to 210 °,
In practice, it may be 180 °. If the predetermined rotation angle is larger than the upper limit of the above range, the fluidity of the sample is excessively reduced and the angular velocity of the thermometer rapidly increases, and it becomes difficult to measure the temperature of the sample at an accurate angular position. When the predetermined rotation angle is smaller than the lower limit of the above range,
This is because the sample is too soft, the angular velocity of the thermometer is small, and the measured value of the temperature varies. In addition, in the results of experiments on various samples, the correlation between the sample measurement temperature measured at a rotation angle in the above range and the softening point according to JIS K2207 is the highest. The softening point measuring device and the softening point measuring method according to the present invention described above can be applied to measure the softening point of any fluid regardless of its type.

[0016]

According to the first aspect of the invention, when the rotating device is started to rotate the rotating plate, at the beginning of rotation, the rotation indicator rod is stationary without rotating in the rotating molten sample, but the sample is cooled. As a result, the fluidity decreases, and the shaft is rotated by being pulled by the rotating sample. Therefore, the temperature when the rotation indicator rod is rotated from the rest position by a predetermined rotation angle, for example, 180 °, is read with a thermometer reading, and is set as the sample measurement temperature. JISK22 corresponding to the sample measurement temperature according to the preset correlation
The softening point according to 07 is calculated.

According to the second aspect of the present invention, a rotation indicator rod is constituted by a thermometer suspended rotatably by a suspender, and a rotation angle of the thermometer is indicated by an indicator thereof. By reading the thermometer reading while visually confirming the rotation angle of the thermometer by looking at the indicator, the softening point measuring device can have a simpler configuration. According to the third aspect of the present invention, since the container is a disposable paper container, there is no need to wash the container, and thus no manual operation is required after the measurement.

[0018]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in more detail with reference to the accompanying drawings. FIG. 1 is a perspective view showing the configuration of one embodiment of the softening point measuring device according to the present invention, and FIG. 2 is a side view of the main part of the softening point measuring device shown in FIG. Softening point measuring device of the present embodiment (hereinafter simply referred to as device) 1
0 denotes a base 12, a gate-shaped support portion 14 standing upright on the base 12, a rotary table 20 that rotates together with a rotary shaft 18 positioned at the center of a line connecting the columns 16A and 16B of the support portion 14,
Rotating device 22 for rotating turntable 20, supporting unit 1
4 comprises a thermometer 26 suspended from an upper extension 24.

The rotary table 20 is formed of a disk member, and has an annular groove on its outer peripheral portion for accommodating a belt in order to fulfill the function of a pulley as described later. Rotary shaft 18
Has a tip fixed to the center (rotation center) of the lower surface of the turntable 20, extends in a direction perpendicular to the turntable 20, and has a lower end pivotally supported by a bearing 28. The bearing 28 is fixed on the base 12. Have been. The rotary table 20 is driven by a rotary device 22 and rotates together with the rotary shaft 18.

The rotating device 22 includes an electric motor 32 driven by a battery 30, a pulley mechanism 34 for transmitting the rotating force of the electric motor 32, and a start switch 36 for the electric motor 32. It is connected. The electric motor 32 is fixed to the column 16A, and its rotation axis is oriented vertically along the column 16A, and the output end is located at the lower end. A battery 30 for driving the electric motor 32 is also removably attached to an appropriate position on the column 16A. Start switch 36
Are provided at appropriate places on the base 12.

The pulley mechanism 34 has a first
A pulley 38, a second pulley 40 coaxially connected to the first pulley 38 and rotating integrally with the first pulley 38 on a lower horizontal plane, and an output end of a rotating shaft of the electric motor 32 and the first pulley 38. A first endless belt 42 stretched between
It comprises a second endless belt 44 stretched between the pulley 40 and the outer periphery of the turntable 20. The shaft connecting the first pulley 38 and the second pulley 40 is supported by conventional means (not shown). The second pulley 40 is arranged at the same height level as the turntable 20, the first pulley 38 is located above the second pulley 40, and the output end of the electric motor 32 has the same height as the first pulley 38. Located on the level. Further, the first belt 42 and the second belt 4
All 4 are made of nylon fishing line.

The thermometer 26 has a temperature measurement range of 30.degree.
A bar-shaped mercury thermometer at a temperature of 00 ° C.
B is suspended from the tip of the extension 24. With such a configuration, the thermometer 26 is rotatable about its longitudinal axis. Further, the thermometer 26 penetrates freely through the upper connecting member 48 and the intermediate connecting member 50 of the support part 14, and descends toward the rotation center of the turntable 20. The thermometer 26 is provided with an angle indicating portion 52 extending parallel to the intermediate connecting member 50 at the rest position so as to slide on the intermediate connecting member 50.

A method for measuring the softening point using the above-described apparatus 10 will be described below with reference to FIGS.
First, a paper disposable cup C having a capacity of 100 cc to 150 cc is prepared, and the molten sample S is put into the cup C so that the thermometer 26 is immersed at a depth of just 28 mm. In order to set the immersion depth of the thermometer 26 to 28 mm, the thermometer 26 may be marked in advance. Next, the cup C containing the sample S is placed on the rotation center of the turntable 20. Then, the electric motor 32 is started by the start switch 36. Thus, the turntable 20 starts rotating with the cup C.
At the beginning of rotation, the sample S in the cup C is molten and has extremely high fluidity, so that the thermometer 26 remains stationary even when the lower portion is immersed in the sample S. However, the sample S is allowed to cool by the rotation of the cup C, and the temperature is lowered to lower the fluidity. Accordingly, the thermometer 26 starts rotating.

The sample temperature at the time when the angle indicating section 50 of the thermometer 26 is rotated by 180 ° is read by the reading of the thermometer 26, and the temperature is recorded as the sample measurement temperature. From the calibration curve (see FIG. 3) showing the correlation between the reading of the thermometer 26 and the softening point according to JIS K2207, the softening point with respect to the above sample measurement temperature is determined, and is set as the softening point of the sample. The calibration curve refers to the measurement of the sample measurement temperature using the above-described apparatus 10 for samples having various different softening points as described above, while measuring the standardized softening point of the same sample according to the method of JIS K2207. This is a graph in which both are correlated, and is created in advance before actual measurement.

Measurement Examples (Examples of Calibration Curves) Various blown asphalt samples having different softening points were measured for the sample measurement temperature by the above-described apparatus 10 as described above, and the softening points of the same samples were determined according to JIS K2207. A calibration curve for the device 10 was created. Rotary table 20
The number of revolutions is 6 rpm, the length of the thermometer 26 is 39.5 cm, the weight is 40 g, and the total length of the pure cotton water thread hanging the thermometer 26 is 50.
cm, thickness was 4th. Rotation angle of thermometer 26 is 1
The temperature at which the temperature reached 80 ° was read by a thermometer 26 as a reading sample measurement temperature. The time required to measure the sample measurement temperature of one sample was about 15 minutes.

The number of samples was 28, and the results were as shown in the graph of FIG. 3. The results of the regression analysis were as follows. In the graph of FIG. 3, the horizontal axis represents the sample measurement temperature, and the vertical axis represents the softening point according to JISK2207. Y intercept 8.6 (correlation coefficient) ² 2.8 X coefficient 0.62 Number of samples 28

As shown in the above-mentioned calibration curve, the sample measurement temperature measured by the apparatus 10 has a satisfactory correlation with the standardized softening point according to JIS K2207, and the sample measurement temperature is measured. Softening point based on JISK
This shows that the value can be sufficiently adopted as an approximate value of the softening point according to 2207.

Using the apparatus 10 of the present embodiment, the sample measurement temperature is measured by the above-described method, and the softening point is determined by the calibration curve, so that the JIS K220 can be used in real time at a manufacturing site, for example, a blown asphalt manufacturing site.
7 can be approximated. As a result, necessary softening point data can be obtained for a sample collected in accordance with the blown asphalt manufacturing process. The present apparatus 10 has a very simple structure and is a small and lightweight apparatus powered by a battery. Since an approximate value of the softening point according to JIS K2207 can be obtained without requiring skill, a skilled tester is required. It is most suitable for simply measuring the softening point at a manufacturing site where there is no waiting.

The configuration of the apparatus 10 of the present embodiment is an example of the softening point measuring apparatus according to the present invention, and the configuration can be modified within the scope of the present invention. For example, the pulley mechanism 34
May be used in place of the gear mechanism, a common universal joint may be used in place of the cotton thread as the suspending tool, and the rotation angle of the thermometer 26 may be measured optically or electrically instead of visually. Further, instead of the rod-shaped thermometer 26, a rotation indicator rod and a digital thermometer may be combined.

[0030]

According to the first aspect of the present invention, when the rotating device is started and the rotating plate is rotated, the rotation indicator rod is pulled by the rotating sample as the fluidity of the sample decreases, and the rotation indicator rod rotates. Therefore, the rotation indicator rod is moved from the stationary position by a predetermined rotation angle,
For example, the temperature at 180 ° rotation is read with a thermometer reading as a sample measurement temperature, and a softening point according to JIS K2207 corresponding to the sample measurement temperature is calculated according to a preset correlation. Thereby, the conventional JISK2207
JISK in a very short time compared to the softening point measurement method
The approximate value of the softening point according to 2207 can be obtained.
Further, the configuration of the apparatus is simple, the production cost is low, and no skill is required for the measurement. As described above, the present softening point measuring device is a measuring device having a simple configuration that can easily measure an approximate value of the softening point.

According to the third aspect of the present invention, since a commercially available disposable paper cup is used as a container for accommodating a sample, washing after measurement is unnecessary. Thereby, the labor required for the measurement can be greatly reduced. According to the fourth aspect of the present invention, the JISK2207 is promptly compared with the conventional JISK2207 softening point measuring method in a very short time.
Since the approximate value of the softening point of the sample can be obtained, it is most suitable for a manufacturing site or the like where the softening point data of the collected sample is required in a short time.

[Brief description of the drawings]

FIG. 1 is a perspective view of an embodiment of a softening point measuring device according to the present invention.

FIG. 2 is a side view of a main part of the softening point measuring device shown in FIG.

FIG. 3 is an example of a calibration curve.

FIG. 4 is a schematic side view showing a configuration of a softening point measuring device according to JIS K2207.

5 (a) is a plan view of a shoulder ring, and FIG. 5 (b) is a cross-sectional view of the shoulder ring taken along the line II ′ of FIG. 5 (a).

6 (a) is a plan view of the shoulder ring, and FIG. 6 (b) is a cross-sectional view taken along the line II-II 'of the ball guide in FIG. 6 (a).

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Example of softening point measuring apparatus 12 Base 14 Support part 16A, B pillar 18 Rotating shaft 20 Rotary table 22 Rotating device 24 Upper extension part 26 Thermometer 28 Bearing 30 Battery 32 Electric motor 34 Pulley mechanism 36 Start switch 38 First Pulley 40 Second pulley 42 First endless belt 44 Second endless belt 46 Hanging tool (thread) 48 Upper connecting member 50 Intermediate connecting member 52 Angle indicating section

Claims (4)

(57) [Claims] 1. A rotating plate for rotating an open container containing a sample whose softening point is to be measured placed on a center of rotation of an upper surface, a rotating device for rotating the rotating plate, and a temperature for measuring the temperature of the sample in the container. A rotation indicator rod that vertically descends into the container, dipped in the sample in the container, and rotates around the longitudinal axis due to adhesion with the sample, and a rotation indicator for measuring the rotation angle of the rotation indicator rod A softening point measuring device comprising a meter. 2. The thermometer is rotatable by a hanger.
Suspended, immersed the lower part in the sample in the container,
A rod-shaped thermometer that measures the temperature of a sample, and
It extends in the direction perpendicular to the longitudinal direction of the thermometer, and
The rotation of a rod-shaped thermometer that rotates around its longitudinal axis
The rotation indicator rod includes an indicator for instructing a rotation angle.
The softening point measuring device according to claim 1, which is a body-forming thermometer . 3. The softening point measuring device according to claim 1, wherein the container is a disposable paper container. 4. An open container containing a molten sample whose softening point is to be measured is placed on the center of rotation of a rotary plate, and a thermometer whose upper part is hung by a hanging string has its longitudinal direction directed to the center of rotation of the rotary plate. In this way, insert the sample into the sample in the container, drive the rotating plate to rotate it, measure the rotation angle of the thermometer with the indicator extending in the direction perpendicular to the longitudinal direction of the thermometer. A method for measuring a softening point of a sample, comprising: measuring a sample temperature at the time of rotating the sample, and obtaining a softening point of the sample based on the sample measured temperature in accordance with a correlation between a previously determined softening point and the sample measured temperature.