JPH05296913A - Measuring instrument for quality of liquid absorbed in solid sample - Google Patents

Abstract

PURPOSE:To obtain an instrument for measuring quantities of liquids absorbed in solid samples which is improved in such a way that the instrument can change a mixed object to slurry and discharge the slurry without allowing the slurry to contaminate the surroundings. CONSTITUTION:The title instrument is constituted principally of a solid sample determinating mechanism, solid sample transferring mechanism, mixing mechanism which mixes the solid sample with a liquid to be absorbed, removing mechanism, and control mechanism and the mixing mechanism is constituted of a mixing chamber 4 incorporating a mixing blade having a rotating speed changing, normally rotating, and reversely rotating functions and provided with an openable upper lid 3 equipped with a nozzle 2 from which the liquid to be absorbed drops at a constant rate. In addition, the mixing blade is provided with a torque detector 5 and the removing mechanism is constituted of a discharging liquid supplying nozzle 6, discharging solution sucking nozzle 7 connected to a pressure reducing system, drying compressed air supplying nozzle 8, and their moving mechanisms 9. The above-mentioned mechanisms are successively operated to perform prescribed operations by means of control signals from the control mechanism.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for measuring the amount of liquid absorbed in a solid sample, and more specifically, a kneaded product after the measurement is made into a slurry and the slurry is removed from the apparatus without contaminating the surroundings. The present invention relates to an improved measuring device.

[0002]

2. Description of the Related Art Conventionally, as a method for measuring a liquid absorption amount of a solid sample, a method is known in which a predetermined liquid is added to a solid sample and mixed, and a change in kneading torque is measured.
For example, in the case of carbon black, the degree of structure, which is one of its physical properties, is indicated by the oil absorption amount, and the oil absorption amount is usually dibutyl phthalate (DB) as a liquid.
P) was used to measure the amount of absorption.

The measuring method utilizing the change of the kneading torque as described above is defined as a mechanical kneading method for carbon black in JIS K 6221 "Test method for carbon black for rubber". The method is as follows. That is, in a kneading chamber of a small mixer called an absorbometer, a liquid sample for absorption (DBP) is kneaded while being added to a certain amount of carbon black at a constant dripping rate, and a change in kneading torque causes a change in carbon black. Measure the oil absorption. After the measurement, the kneaded material in the kneading chamber is removed, and the material is prepared for the next measurement.

[0004]

In the above measuring method, the working efficiency depends on the removal of the kneaded material after the measurement, but since the kneaded material exhibits clay-like properties,
Its removal is extremely difficult. Further, it is necessary to manually disassemble the kneading chamber and clean the inside every time the measurement is performed, and the operability is extremely poor. The applicant has previously constructed a kneading chamber as a structure capable of assembling and disassembling a liquid absorption amount of a solid sample, and after the measurement, supplies a liquid for removal such as water to the kneading chamber for kneading. A kneading chamber was decomposed after the kneaded material in the room was made into a slurry state, and then an improved measuring device was proposed so that the slurry could be discharged from the kneading chamber by air blow (Japanese Patent Application No. 2-257953).

In the above measuring device, although the kneading chamber is automatically cleaned, the operability is remarkably improved.
Since the air is blown into the kneading chamber, there is a disadvantage that the slurry scatters and stains the surroundings. The present invention has been made in view of the above circumstances, and its object is to make a kneaded product after the measurement into a slurry, and a measuring device improved so that the slurry is removed from the device without polluting the surroundings. To provide.

[0006]

That is, the gist of the present invention is to knead while adding a predetermined liquid to be absorbed at a constant drip rate to a fixed amount of solid sample, and by changing the kneading torque,
A device for measuring a liquid absorption amount of a solid sample, comprising:
The solid sample quantification mechanism (A), the solid sample transfer mechanism (B), the kneading mechanism (C) for the solid sample and the liquid to be absorbed, the removing mechanism (D), and the control mechanism (E) are mainly configured. C) has a kneading blade (1) having a variable rotation speed function and both forward and reverse rotation functions, which is disposed inside, and an openable and closable upper lid (2) provided with a liquid constant velocity dropping nozzle (2) for absorption. 3) having a kneading chamber (4), the kneading blade (1) includes a torque detector (5), and the removing mechanism (D) includes a removing liquid supply nozzle (6), It is composed of a removal suction nozzle (7) connected to a decompression system, a drying compressed air supply nozzle (8), and a moving mechanism (9) for these, and each of the above mechanisms is controlled by a control mechanism (E). The solid sample liquid characterized by performing the following operations in sequence by the control signal of It resides in the absorption amount of the measuring device. The solid sample quantification mechanism (A) collects a fixed amount of solid sample. The solid sample transfer mechanism (B) supplies the collected solid sample into the kneading chamber (4) whose upper lid (3) is open. The kneading mechanism (C) closes the upper lid (3), starts driving the kneading blade (1), and supplies the liquid to be absorbed into the kneading chamber (4) from the liquid to be absorbed constant velocity dropping nozzle (2). Drip for a period of time and open the top lid (3). The removal mechanism (D) is moved to the upper part of the kneading chamber (4) with the upper lid (3) opened, and is used for slurrying the kneaded product from the removal liquid supply nozzle (6) into the kneading chamber (4). Supply the required amount of removal liquid. The kneading mechanism (C) changes the kneading blade (1) to a high-speed rotation and rotates the kneading blade (1) forward and backward at regular intervals. The removal mechanism (D) sucks and removes the slurry in the kneading chamber (4) through the removal suction nozzle (7), and then the compressed compressed air for drying enters the kneading chamber (4) from the compressed air supply nozzle (8) for drying. Is supplied for a predetermined time. The kneading mechanism (C) stops driving the kneading blade (1).

[0007]

Embodiments of the present invention will be described below with reference to the accompanying drawings. 1 to 6 are explanatory views showing an example of the measuring apparatus of the present invention, and FIG. 1 is a kneading mechanism (C) in which the solid sample transfer mechanism (B) and the upper lid (3) of the measuring apparatus of the present invention are omitted.
2 is a kneading mechanism (C) of the measuring device of the present invention.
3 is a kneading mechanism (C) of the measuring device of the present invention.
FIG. 4 to FIG. 4 are partial explanatory views mainly showing the solid sample quantification mechanism (A) of the measuring apparatus of the present invention.

The measuring apparatus of the present invention comprises a solid sample quantification mechanism (A), a solid sample transfer mechanism (B), a kneading mechanism (C) for a solid sample and a liquid to be absorbed, a removal mechanism (D) and a control mechanism ( It is mainly composed of E).

The solid sample quantification mechanism (A) has a through hole (1
3) a turntable (14), a turntable driving device (15), a solid sample container (16), a balance (1
7) and a load placing member (18). And the solid sample quantification mechanism (A), as a preferred embodiment,
Includes solid sample table (19) and solid sample feeder (20) for coarse weighing.

The solid sample table (19) supplies a plurality of solid samples mounted thereon to the container (16) on the turntable (14) in a predetermined order. The driving of the solid sample table (19) is controlled by a feeding mechanism (not shown), and is performed in accordance with the driving state of the turntable (14). Then, the supply amount of the solid sample is determined by the balance (1
It is weighed in 7) and the supply is stopped when the supply amount reaches a preset value. An alarm device (not shown) that issues an alarm signal when the supply amount exceeds the set value is preferably attached to the balance.

According to the embodiment shown in FIG. 5, the through hole (1
When placing the container (16) on top of (3), the container (1
A suitable container holder (21) is provided around the through hole (13) so that the center of 6) and the center of the through hole (13) coincide with each other.
Is preferably provided. On the other hand, according to the aspect shown in FIG. 6, when the container (16) is housed in the through hole (13), for example, the container (16) is prevented from falling from the through hole (13). A suitable retainer (22) must be provided around the circumference of the.

The weighing of the solid sample is performed by supporting the container (16) on the load placing member (18). This supporting state is achieved by vertically moving either the turntable (14) or the load placing member (18). Therefore, the turntable (14) and the load placing member (18) are arranged so that the container (16) can be supported either by the turntable (14) or by the load placing member (18). )
A mechanism (not shown) for moving the and relative to each other in the vertical direction is provided on either the turntable (14) or the balance (17). The above mechanism is preferably provided on the balance from the viewpoint of simplification. Further, the through hole (13) is provided in the container (16) depending on the shape and weighing mode of the container (16).
It is necessary that at least one of the load mounting member (18) and the load mounting member (18) be configured to be movable back and forth.

The solid sample transfer mechanism (B) comprises a solid sample input arm (23) and a guide rail (24). The solid sample charging arm (23) has a gripping part at its tip end that is rotatable by a control mechanism (not shown), and the gripping part grips the container (16).

The guide rail (24) is connected to the drive unit main body (1).
0) is fixed to the upper part, and an appropriate moving mechanism (not shown) is provided inside thereof. The solid sample loading arm (23) is supported perpendicularly to the guide rail (24) and can be moved left and right by a moving mechanism inside the guide rail (24). In addition, in FIG. 1, the drive unit main body (10) is illustrated with the ceiling part omitted to show the inside thereof, but in reality, the ceiling part is provided and the guide part is provided on the ceiling part. The rail (24) is fixed.

The kneading mechanism (C) is provided with a kneading blade (1) having a variable rotation speed function and a forward / reverse rotation function, and a liquid constant speed dropping nozzle (2) for absorption. It comprises a kneading chamber (4) having an openable and closable upper lid (3). The kneading blade (1) is supported by the side wall of the drive unit main body (10) and is housed inside the motor (12).
Is rotated by. A torque detector (5) is provided in the power transmission system (11) of the kneading blade (1).

A kneading blade that rotates only in one direction may be used for measuring the liquid absorption amount, but a removing mechanism (D) described later is used.
In order to efficiently suck and remove the slurry in the kneading chamber (4) by means of the kneading chamber (4), the kneading blade (6) having both forward and reverse rotation functions is provided.
Is required. Further, it is necessary to change the rotation speed of the kneading blade (6) to rotate the kneading blade (6) at a high speed.

The upper lid (3) is openable / closable by a foldable structure, and is opened / closed by the upper lid opening / closing motor (3 ') centering on the end portion on the drive unit main body (10) side. The liquid to be absorbed constant speed dropping nozzle (2) is provided in the upper lid (3), and the dropping port thereof faces the dropping hole (2 ′) provided in the upper lid (3). Further, the liquid constant velocity dropping nozzle (2) for absorption has a bent shape so as not to interfere with the opening and closing of the upper lid (3). An automatic buret, a metering pump, or the like is used as the absorbed liquid constant velocity dropping nozzle (2).

The removing mechanism (D) includes a removing liquid supply nozzle (6), a removing suction nozzle (7) connected to a decompression system (not shown), a drying compressed air supply nozzle (8), and these. It is composed of a moving mechanism (9). Each of the above nozzles is fixedly mounted on a moving plate (9 ') that can be moved up and down by a moving mechanism (9). The tip opening of each nozzle is formed on the back side surface of the moving plate (9 ').

The removing mechanism (D) is arranged above the kneading chamber (4). When removing the slurry in the kneading chamber (4), the moving mechanism (9) lowers the upper lid (3) to the upper part of the kneading chamber (4) which is opened. As a result, the moving plate (9 ') comes into contact with the top of the side wall of the kneading chamber (4). The size of the moving plate (9 ') is slightly smaller than the area of the upper open space part of the kneading chamber (4) so that when it comes into contact with the top of the side wall of the kneading chamber (4), voids are formed on both sides thereof. Good to do. When the slurry in the kneading chamber (4) is sucked and removed through the suction nozzle for removal (7), the above-mentioned gap acts so that ambient air is sucked into the suction nozzle for removal (7). Then, the slurry in the kneading chamber (4) is sucked up into the removal suction nozzle (7) at once by the flow of the air sucked into the removal suction nozzle (7).

The control mechanism (E) (not shown) comprises a publicly known control means such as a relay sequence, a sequencer, a personal computer, etc., and gives a predetermined control signal to each of the above mechanisms. As a result, the above-mentioned mechanisms sequentially perform the following operations 1 to. Then, each operation is automatically performed by a control signal including an ON-OFF control signal by a timer.

The solid sample quantification mechanism (A) collects a fixed amount of solid sample. When measuring the oil absorption of carbon black, the collected amount is usually about 20 g. The solid sample transfer mechanism (B) supplies the collected solid sample into the kneading chamber (4) whose upper lid (3) is open.

The kneading mechanism (C) closes the upper lid (3), starts driving the kneading blade (1), and absorbs the liquid to be absorbed into the kneading chamber (4) from the liquid constant-velocity dropping nozzle (2) for absorption. The liquid is dripped for a predetermined time, and the upper lid (3) is opened. The change of the kneading torque is performed by the torque detector. Then, for example, the addition amount of the absorbed liquid corresponding to 70% torque of the maximum torque is obtained, and the addition amount of the absorbed liquid per unit weight of the solid sample is calculated from this, and this is calculated as It can be a liquid absorption amount.

The removal mechanism (D) is moved to the upper part of the kneading chamber (4) whose upper lid (3) is opened, and the kneaded product is discharged from the removal liquid supply nozzle (6) into the kneading chamber (4). An amount of removing liquid necessary for slurrying is supplied. The supply amount of the removing liquid is not particularly limited, but is usually in the range of 0.5 to 2.0 times the weight of the solid sample. For example,
Measurement of oil absorption of carbon black described above (collected amount of about 2
In the case of 0 g), about 100 ml is sufficient as the supply amount of the removing liquid. Then, the added removing liquid is mixed with the kneaded material in the kneading chamber, and the mixing time is sufficient for 1 to several minutes. Then, the kneaded material in the kneading chamber becomes a slurry and loses a clay-like property when mixed with the removing liquid.

The kneading mechanism (C) changes the kneading blade (1) to a high-speed rotation and rotates the kneading blade (1) forward and backward at regular intervals. For example, 10 to 9 at a rotation speed of 150 to 250 rpm.
Drive for 0 seconds, forward and reverse two times each,
It is preferable to repeat 4 times or more. Specifically, in the case of measuring the oil absorption of carbon black described above, if the kneading blade (1) is rotated at a high speed at a double speed at the time of measurement, the forward and reverse rotations are switched every 10 seconds and driven for about 1 minute. Good.

The removal mechanism (D) sucks and removes the slurry in the kneading chamber (4) through the removal suction nozzle (7) and then dries it into the kneading chamber (4) through the drying compressed air supply nozzle (8). Supply compressed air for a predetermined time. The suction force of the removal suction nozzle (7) is usually 5000 to 900.
It may be about 0 mmH ₂ Oabs. The suction operation allows the slurry in the kneading chamber (4) to be satisfactorily removed to the outside of the system. In particular,
Even during the suction operation, since the kneading blade (1) is driven, it is possible to remove the slurry over the details in the kneading chamber (4). The compressed air for drying is not applied to wipe and remove the slurry in the kneading chamber (4), but is used to dry the inside of the kneading chamber (4).
Therefore, it is not necessary to use strong compressed air,
Also, the amount does not have to be large. The use of high-temperature air is preferable in order to improve the drying efficiency.

In the measuring apparatus of the present invention, the target solid sample is powder or granules, of which carbon black is a typical example, but pigments such as alumina, silica and titania, and other solid samples can also be mentioned. The liquid to be absorbed is arbitrarily selected depending on the type of solid sample and the purpose of measurement. For example, in carbon black, dibutyl phthalate (DBP) is used when evaluating the degree of its structure. Water is usually used as the removing liquid. The measuring device of the present invention is a mechanical kneading method (JIS K) specified for carbon black.
6221) can be suitably used.

[0027]

According to the present invention described above, a kneaded material after completion of measurement is made into a slurry, and an improved measuring device is provided so that the slurry can be removed from the device without polluting the surroundings. According to the measuring device of the invention, the liquid absorption amount of a solid sample can be efficiently measured. Therefore,
The industrial value of the present invention is great.

[Brief description of drawings]

FIG. 1 is an explanatory view of a kneading mechanism (C) in which the solid sample transfer mechanism (B) and the upper lid (3) of the measuring apparatus of the present invention are omitted.

FIG. 2 is an explanatory diagram of a kneading mechanism (C) of the measuring device of the present invention.

FIG. 3 is an explanatory diagram of a kneading mechanism (C) and a removing mechanism (D) of the measuring device of the present invention.

FIG. 4 is a partial explanatory view mainly showing a solid sample quantification mechanism (A) of the measuring apparatus of the present invention.

FIG. 5 is a partial explanatory view mainly showing a solid sample quantification mechanism (A) of the measuring apparatus of the present invention.

FIG. 6 is a partial explanatory view mainly showing a solid sample quantification mechanism (A) of the measuring apparatus of the present invention.

[Explanation of symbols]

 1: Kneading blade 2: Liquid constant velocity drip nozzle for absorption 2 ': Dripping hole 3: Top lid 3': Top lid opening / closing motor 4: Kneading chamber 5: Torque detector 6: Removal liquid supply nozzle 7: Removal suction nozzle 8: Drying compressed air supply nozzle 9: Moving mechanism 9 ': Moving plate 10: Drive unit main body

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Shinichi Kanamaru 1-1 Kurosaki Shiroishi, Hachimansai-ku, Kitakyushu, Fukuoka Prefecture Mitsubishi Kasei Co., Ltd. Kurosaki Plant

Claims (1)

[Claims] 1. A device for measuring a liquid absorption amount of a solid sample by changing a kneading torque by kneading a predetermined amount of a liquid to be absorbed with a predetermined liquid to be absorbed at a constant dropping rate. A solid sample quantification mechanism (A), a solid sample transfer mechanism (B), a kneading mechanism (C) for mixing the solid sample with the liquid to be absorbed,
The kneading mechanism (C) mainly includes a removing mechanism (D) and a control mechanism (E), and the kneading blade (1) having a variable rotation speed function and both forward and reverse rotation functions is arranged inside. It is composed of a kneading chamber (4) having an openable and closable upper lid (3) equipped with a liquid constant velocity liquid dropping nozzle (2) for absorption, and further, the kneading blade (1) is provided with a torque detector (5). The removal mechanism (D) includes a removal liquid supply nozzle (6), a removal suction nozzle (7) connected to a decompression system,
It is composed of a compressed air supply nozzle (8) for drying and a moving mechanism (9) for these, and each of the above mechanisms sequentially performs the following operations in accordance with a control signal from the control mechanism (E). An apparatus for measuring a liquid absorption amount of a solid sample, characterized in that: The solid sample quantification mechanism (A) collects a fixed amount of solid sample. The solid sample transfer mechanism (B) supplies the collected solid sample into the kneading chamber (4) whose upper lid (3) is open. The kneading mechanism (C) closes the upper lid (3), starts driving the kneading blade (1), and supplies the liquid to be absorbed into the kneading chamber (4) from the liquid to be absorbed constant speed dropping nozzle (2). Drip for a period of time and open the top lid (3). The removal mechanism (D) is moved to the upper part of the kneading chamber (4) with the upper lid (3) opened, and the kneaded product is slurried from the removal liquid supply nozzle (6) into the kneading chamber (4). Supply the required amount of removal liquid. The kneading mechanism (C) changes the kneading blade (1) to a high-speed rotation and rotates the kneading blade (1) forward and backward at regular intervals. The removal mechanism (D) sucks and removes the slurry in the kneading chamber (4) through the removal suction nozzle (7), and then the compressed compressed air for drying enters the kneading chamber (4) from the compressed air supply nozzle (8) for drying. Is supplied for a predetermined time. The kneading mechanism (C) stops driving the kneading blade (1).