JP3326220B2 - Rotational viscometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a rotational viscometer for measuring viscosity.

[0002]

2. Description of the Related Art Conventionally, this type of rotational viscometer has a rotating container for accommodating a sample, and a torque detector inserted into the sample in alignment with the axis of the rotating container. Accordingly, a configuration is adopted in which the torque detector detects the viscous force received from the sample as torque and measures the viscosity of the sample. By the way, as an application of such a rotational viscometer,
In addition to the measurement of a fluid that is in a fluid state at normal temperature, there is also a case in which a fluid exhibits a solid phase at normal temperature and shows a liquid phase at an elevated temperature. That is, it may be necessary to confirm the viscosity of slag, glass, or the like, or a mixture thereof in a high-temperature molten state, for the purpose of, for example, favorably pouring a melt such as incineration ash from a furnace. Conventionally, when measuring the viscosity of such substances, the point of change from the solid phase to the liquid phase for each object to be measured is determined empirically and experimentally (by grasping the melting state associated with the temperature rise operation of the sample). Experiment), the sample temperature measurable by the rotational viscometer was set in advance, and the viscosity was measured.

[0003]

However, the above-mentioned prior art has the following problems since individual measurers judge the sample temperature from the solid phase to the liquid phase of the sample. (1) The criterion for determining the minimum temperature of a sample in a fluid state where the viscometer can measure the viscosity varies, and the criterion is not constant. (2) As a result, since the above-mentioned minimum temperature tends to be set on the safe side of the viscometer, it is difficult to measure the viscosity in a high viscosity state where the sample is on the low temperature side. (3) Since the temperature at which the solid phase changes to the liquid phase cannot be accurately measured, if the above-mentioned minimum temperature is set low, the sample is solidified in the viscosity measurement during the temperature lowering operation, and the rotation mechanism of the viscometer is used. Parts may be damaged. (4) Further, since the low temperature limit temperature is unknown,
It is difficult to automate the measurement even when it is desired to measure the viscosity while alternately repeating the temperature decrease. In addition, when the viscosity is to be accurately measured in a high viscosity state, it is necessary for the measurer to check the state of the sample while checking the state of the sample one by one.

Accordingly, an object of the present invention is to make it possible to determine the molten state of a sample based on a certain standard, and as a result, to set the lowest measurable temperature allowed for a viscometer from a reasonable standard and to automatically measure the temperature. To obtain a rotational viscometer that enables

[0005]

The rotary viscometer according to the present invention for achieving the above object has a characteristic configuration comprising: urging means for urging a torque detecting portion into the sample from outside the sample; Heating means for raising and melting the temperature, and a judging means for judging whether or not the viscosity can be measured by detecting the melting state of the sample based on the positional relationship between the torque detector and the sample. It is as follows.

[0006]

The rotary viscometer of the present application has a biasing means, a heating means,
A determination means is provided. When the sample to be measured is a sample that melts in a heated state, the torque detecting unit is urged by the urging means from the outside of the sample in contact with the sample and held. Then, when the sample is softened by the action of the heating means and comes into a flowing state, the torque detector enters the sample. The intrusion state is detected by the discriminating means as a positional relationship between the torque detector and the sample, and when the intrusion is completed, it is determined whether or not the sample is in a molten state, and it is determined whether or not viscosity measurement can be performed according to the molten state. Is done. Therefore, the change in viscosity of the sample in its molten state is determined based on a certain standard, and it is reliably detected whether or not the sample is in a state where the measurement of viscosity is permitted to be started, and is used for the subsequent measurement operation.

[0007]

Therefore, the following effects can be obtained. (1) Since the change of the sample from the solid phase to the liquid phase can be detected and set, the molten state determined by the discriminating means (confirmation of the highest viscosity at which the viscosity can be measured) is effectively used, and the viscosity is measured in this state. Is started, the measurement start viscosity becomes almost constant, and a relatively wide range of viscosity from low temperature to high viscosity can be measured. (2) Measurable By setting the molten state appropriately, the measurement can be performed without solidifying the sample even at the time of high viscosity measurement, and the rotation function unit and the like are not damaged. (3) Since the measurable melting state can be known by, for example, the measurement start temperature, it is possible to automate a rotational viscometer capable of responding to all kinds of samples, thereby relieving the operator of complicated work. I was able to. Further, if the amount of movement of the torque detecting unit accompanying the temperature raising operation of the sample from the solid phase to the liquid phase is monitored, the melting characteristics of the sample (JIS K 2151, JI
SM 8801, the test method for cokes and coals) can be known from the amount of movement of the torque detection unit, and the melting characteristics and viscosity of the sample can be simultaneously checked.

[0008]

An embodiment of the present invention will be described with reference to the drawings. FIG. 1A is a front view of the rotational viscometer of the present application, and FIG. 1B is a plan view thereof. The rotational viscometer according to the present application generally includes a sample unit 100 in which a sample 1 is accommodated and measured, and a measuring unit that is immersed in the sample 1 and measures a viscous force received by the torque detecting unit 2 from the sample 1. 200.

Hereinafter, each of the parts will be described. The sample unit 100 includes a rotating container 3 in which the sample 1 is placed, a rotating shaft 4 connected to the rotating container 3, and a motor 5 attached to the other end of the rotating shaft 4. Therefore, this portion 100 is rotated by the motor 5 at a constant speed.
This is for giving rotation to the sample 1 inside. A moving mechanism 30 for moving the rotating container 3 in the vertical direction of the machine base;
The torque detecting unit 2 and the rotating container 3 are provided.
The vertical relative position with respect to is settable. Further, a temperature detecting means 500 for measuring the temperature of the sample in the rotating container 3 is provided.

Next, the measuring section 200 will be described. This part 200 is a part for detecting and measuring the viscous force applied to the torque detector 2 immersed in the sample 1. As shown in the figure, a torque transmitting shaft 6 is connected to the torque detecting section 2, and the other end of the torque transmitting shaft 6 is supported by bearings 7 and 7 in a double-supported state. Here, the rotating shaft 4 of the sample 1 and the torque transmitting shaft 6 are set concentrically. Further, a torque transmitting shaft 6 is provided between the bearings 7 forming a support structure.
And a disc-shaped connecting portion 8 is provided integrally therewith. Now, a tensioned metal wire 9 is connected to the connecting portion 8 by a circumferential portion 8a. One end of the metal wire 9 is connected to the detection unit 11 having the load cell 10, and the other end is supported by a pulley 12 so as to hold the metal wire 9 horizontally, and a weight 13 is hung at the tip. Have been. By employing this structure, an appropriate tension is applied to the metal wire 9 in advance as described above, and the tension of the metal wire 9 is maintained. Further, the load cell 1 provided in the detection unit 11 described above.
0 is connected to the load cell 14 for detecting the distortion of the load cell 10. The above-described torque detection unit 2, torque transmission shaft 6, connection unit 8, and metal wire 9 are configured to be movable in the vertical direction as illustrated in FIG. 4, and in order to secure the measurement position illustrated in FIG. Stopper 61 between the main body
It is configured with. Further, the machine body 50 described above is provided with a differential transformer 51 as a position detecting means.
The vertical position of the torque transmission shaft 6 can be detected by the transformer 51. Here, the direction of the sample placed in the rotating container 3 by gravity (downward) is the torque detecting unit 2.
This configuration is called biasing means. The above is the structure of the rotational viscometer. By adopting the above structure, the viscous force applied to the torque detector 2 due to the viscosity of the sample 1 is transmitted to the load cell 11 without energy loss, and the viscosity of the sample 1 is measured. Is done.

An electric furnace 52 as a heating means for setting the temperature of the sample contained in the rotating container 3 is provided by:
It is provided around the sample unit 100. The electric furnace 52 is configured to be vertically movable with respect to the rotating container 3 by a unique driving mechanism 53.

The measurement is controlled by the controller 501 based on the position of the torque transmission shaft 6 (the vertical position of the torque detector 2 with respect to the sample 1) detected by the differential transformer 51 and the sample temperature. Is done. This control device 5
01 includes a determination unit 502 and a melting information detection unit 503. That is, the determination means 502 detects the molten state of the sample based on the positional relationship between the torque detector 2 and the sample 1, and determines whether or not the viscosity can be measured. When the determination unit 502 determines that the sample 1 is in a molten state, the rotation container 3 starts rotating and the viscosity measurement of the sample 1 is started. On the other hand, based on the information detected by the temperature detecting means 500 and the position detecting means 51, the melting information detecting means 503 determines the melting characteristics (softening point, softening point, (Correlation chart of melting point, melting point, position of torque detector 2 accompanying temperature rise and temperature, etc.)
Is what you get. For example, as to the softening point and the melting point of the sample 1, the moving amount of the softening point and the moving point of the melting point are set in advance as the moving amount of the torque detecting unit 2, and the moving amount of the softening point and the melting point of the torque detecting unit 2 are set in advance. Each temperature of the sample 1 moved by the amount is determined as the softening point and the melting point of the sample. Hereinafter, the operation of the rotational viscometer will be described with reference to the flow shown in FIG. 1 Start of a measurement operation 2 A sample 1 whose viscosity is to be measured is accommodated in a rotating container 3, and the rotating container 3 is mounted on a rotating shaft 4 attached to a motor 5.
Set to. Before the start of the measurement, the sample 1 is in a solid state. 3 Input measurement conditions to the controller 501. Here, the measurement conditions are the immersion depth (insertion depth) of the torque detector 2 into the sample 1 and the temperature pattern at the time of measuring the viscosity (an example of this temperature pattern is shown in FIG. 3. In FIG. Indicates the time, and the vertical axis indicates the sample temperature. In this pattern, linear temperature decrease and increase are performed once each), the maximum measured temperature, the minimum measured temperature, and the like. 4 Raise the rotating container 3 to start measurement. 5 While observing the state of contact between the sample surface 1a and the lower end 2a of the torque detector, the ascending operation is performed until they come into contact. 6 Predetermined immersion depth (insertion depth) from the above position
Then, the rotating container 3 is lifted to complete the raising operation of the rotating container 3. FIG. 4A shows a state in which the ascending has been completed. 7. The electric furnace 52 is set at a predetermined position, and the temperature of the sample 1 is raised. 8. When the temperature of the sample 1 increases and the sample 1 starts to soften, the torque detector 2 gradually falls into the sample 1 by its own weight. 9 The amount of softening point movement set in advance is
When 1 is detected, the temperature of the sample 1 at this time is determined as the softening point. 10 The differential melting point 5
When 1 is detected, the temperature of the sample 1 at this time is determined as the melting point. 11 The rotation of the rotary container 3 is started in a state where the stopper 61 comes into contact with the apparatus main body 50 and the torque detector 2 comes to the position shown in FIG. 4B (the related position shown in FIG. 1). The temperature of the sample 1 in this state is set as the measurable limit temperature. 12 In this state, the torque detector 2 is set at the measurement position, and the viscosity measurement can be started. 13 In measuring the viscosity, the above-mentioned input measurement conditions are referred to. Here, the minimum measured temperature on the input side and the measurable limit temperature determined by the apparatus itself through the above-described process are conditioned so that the minimum measured temperature on the input side does not fall below the measurable limit temperature. 14 When the predetermined measurement pattern is completed, the measurement is finished, and the electric furnace 52 is stopped. 15 Finish measuring work

Therefore, the measurement of the viscosity by the rotational viscometer achieves complete automation except for the accommodation of the sample in the rotating container.

[Alternative Embodiment] In the above embodiment, the case where the metal wire 9 is used for connecting the load cell 10 and the connecting portion 8 has been described. May be employed. Also, in order to handle samples having different viscosities, a load cell 1
0, or connect the disc-shaped connecting portion 8 to the torque transmitting shaft 6,
The measurement range can be changed by changing the diameter of the disc-shaped connecting portion 8 so that it can be exchanged and connected to the metal wire 9.

In the claims, reference numerals are provided for convenience of comparison with the drawings, but the present invention is not limited to the configuration shown in the accompanying drawings.

[Brief description of the drawings]

FIG. 1 is a diagram showing a configuration of a viscometer.

FIG. 2 shows a measurement sequence.

FIG. 3 is a diagram showing a temperature state of a sample over time.

FIG. 4 is an explanatory diagram of a viscosity measurement state.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Sample 2 Torque detection part 3 Rotating container 51 Position detection means 52 Heating means 500 Temperature detection means 502 Judgment means 503 Melting information detection means

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-55-122135 (JP, A) JP-T-63-501097 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) G01N 11/00-11/16 JICST file (JOIS)

Claims (5)

(57) [Claims] 1. A rotating container (3) for accommodating a sample (1), and a torque detector (2) that can be inserted into the sample (1) in accordance with the axis of the rotating container (3), With the torque detector (2) inserted into the sample (1), the torque detector (2) is rotated with the rotation of the rotating container (3).
Is a rotational viscometer for measuring the viscosity of the sample (1) by viscous force received from the sample (1), wherein the torque detector (2) enters the inside of the sample from outside the sample (1). An urging means for energizing, and a heating means (52) for raising / melting the sample (1) are provided, and the sample is melted according to a positional relationship between the torque detector (2) and the sample (1). A rotational viscometer provided with a determining means (502) for detecting a state and determining whether or not viscosity measurement is possible. 2. When the determination means (502) determines that the sample (1) is in a molten state, the rotation of the rotating container (3) is started to start measuring the viscosity of the sample (1). The rotational viscometer according to claim 1, wherein 3. The rotation according to claim 1, wherein the urging means causes the torque detector (2) to enter the sample (1) by the action of gravity as the temperature of the sample rises and melts. Viscometer. 4. A temperature detecting means (500) for measuring a temperature of the sample (1) and a position detecting means (51) for detecting a position of the torque detecting section (2) with respect to the sample (1), 2. The rotational viscometer according to claim 1, further comprising: melting information detecting means (503) for obtaining melting characteristics of the sample (1) from a relationship between a movement amount of the torque detecting unit (2) and a temperature of the sample (1). . 5. The softening point and the melting point of the sample are set as the melting characteristics, and the softening point shift and the melting point shift are set in advance as the shift amounts, and the torque detecting unit (2) sets the softening point shift. The rotational viscosity according to claim 4, wherein the melting information detecting means (503) is configured to determine each temperature of the sample (1) moving by an amount and a melting point shift amount as a softening point and a melting point of the sample. Total.