Absorption amount evaluation method and absorption amount evaluation system

Abstract

To provide a technique for performing an elimination process more efficiently and carefully at low costs while obtaining a correct evaluation result in evaluation of the amount of absorption.SOLUTION: An absorption amount evaluation method includes: a first preparation process of throwing a sample into a mixing container having an agitation section; a measurement process of measuring resistance generated with the agitation section during mixture by a first mixed sample in a mixing container obtained by mixing while adding a first solvent to the sample; an evaluation process for obtaining the amount of absorption of the sample from the resistance value; a second preparation process of throwing a solvent absorbent into the first mixed sample in the mixing container; a reaction process of obtaining a second mixed sample by mixing the first mixed sample and the solvent absorbent; an elimination process of eliminating the second mixed sample from the mixing container by performing breaking and suction by spraying gas to the second mixed sample; and a cleaning process of cleaning the mixing container by performing suction while spraying a second solvent to the mixing container after the elimination process.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a method for evaluating absorption amount and an absorption amount evaluation system.

Background Art

[0002] Powder materials include carbon powder, pigment powder, catalyst powder, and ceramic powder, as well as single metal powder, metal compound powder, metal oxide powder, and metal hydroxide powder. They widely exist from raw materials to products in various industries, including the fields of electronic devices, catalysts, and batteries. Recently, research and development of functional materials such as nanoparticles and porous bodies have been actively promoted, and clarifying their characteristics has extremely important significance. As methods for evaluating these, qualitative analysis, quantitative analysis, and state / structure analysis by chemical analysis methods and physical analysis methods can be mentioned. For example, measurement of the absorption amount (oil absorption amount, water absorption amount, etc.) is also counted as one of the indispensable methods for grasping the characteristics of powder materials.

[0003] Among them, the oil absorption amount is also referred to as the "oil absorption capacity". For example, in "JIS_K_6217-4:2008_Carbon Black for Rubber - Basic Characteristics - Part 4: Method for Determining Oil Absorption Amount (Including Compressed Sample)", the method for determining the oil absorption amount using an absorptometer is described among the basic characteristics of carbon black used as a rubber compounding agent. In recent years, absorption amount measuring devices conforming to the above JIS, that is, after putting the carbon black to be measured into a mixing cell attached with a rotating blade, while adding oil little by little and stirring, detecting the resistance (torque) signal applied to the rotating blade caused by the thickening of the carbon black that has absorbed the oil, such as absorption amount measuring instruments S410D, S410E, and S-500 (manufactured by Asahi Riken Co., Ltd.), oil absorption amount liquid absorbers Absorptometer A, B, C, and E (Germany: Brabender GmbH & Co. KG), DABS oil absorber (Luxembourg: Hit Exur Luxembourg Co., Ltd.), etc. have been put on the market.

[0004] By the way, the prior art regarding the above absorption amount evaluation method is disclosed as follows. Patent Document 1 discloses: (1) In a kneading chamber, while kneading a fixed amount of solid sample by adding a predetermined liquid to be absorbed at a constant dropping rate, a method for measuring the liquid absorption amount of the solid sample based on the change in kneading torque. After the measurement is completed, when discharging and removing the mixture in the kneading chamber from the kneading chamber, a removing liquid with a difference of 3 or more from the solubility parameter (cal / cm 3 L) 1 / 2 of the solid sample and / or the liquid to be absorbed is added and mixed in advance. A method for measuring the liquid absorption amount of a solid sample, and (2) an apparatus for measuring the liquid absorption amount of a solid sample by kneading while adding a predetermined liquid to be absorbed to a fixed amount of solid sample at a constant dropping rate and measuring the change in kneading torque. The apparatus mainly consists of a solid sample metering mechanism (A), a solid sample transfer mechanism (B), a kneading mechanism (C) for the solid sample and the liquid to be absorbed, and a control mechanism (D). The kneading mechanism (C) is configured to be disassembled and assembled by the movement of the outer wall, and a kneading blade (6) equipped with a torque detector (5) is arranged inside. It is mainly composed of a kneading chamber (4), a compressed air supply nozzle (1) arranged above it, a constant-speed dropping nozzle (2) for the liquid to be absorbed, and a supply nozzle (3) for the removing liquid. Then, according to the control signal from the control mechanism (D), the solid sample metering mechanism (A) collects a fixed amount of solid sample, the solid sample transfer mechanism (B) supplies the collected solid sample to the kneading chamber (4) of the kneading mechanism (C), and the kneading mechanism (C) drives the kneading blade (6) and allows the liquid to be absorbed to drop from the constant-speed dropping nozzle (2) for the liquid to be absorbed for a predetermined time, then stops the dropping. Next, after supplying the required amount of the removing liquid from the supply nozzle (3) for the removing liquid, it stops the supply. Then, it moves the outer wall constituting the kneading chamber (4) to disassemble the kneading chamber and discharge and remove the internal mixture. Next, after supplying compressed air from the compressed air supply nozzle (1) for a predetermined time, it stops the supply and stops the drive of the kneading blade (6). Then, it moves the outer wall to assemble the kneading chamber (4). A measuring apparatus for the liquid absorption amount of a solid sample is disclosed.

[0005] Next, Patent Document 2 discloses an apparatus for measuring the liquid absorption amount of a solid sample by kneading while adding a predetermined liquid to be absorbed to a certain amount of the solid sample at a constant dropping rate, and measuring the change in kneading torque. The apparatus mainly comprises a solid sample metering mechanism (A), a solid sample transfer mechanism (B), a kneading mechanism (C) for the solid sample and the liquid to be absorbed, a removal mechanism (D), and a control mechanism (E). The kneading mechanism (C) is configured with a kneading chamber (4) having an upper lid (3) that can be opened and closed and is provided with a constant-speed dropping nozzle (2) for the liquid to be absorbed, and a kneading blade (1) having a variable rotation speed function and a forward and reverse rotation function is arranged inside. Moreover, the kneading blade (1) is provided with a torque detector (5). The removal mechanism (D) is composed of a removal liquid supply nozzle (6), 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 performs the operations described in Table 1 below in numerical order according to a control signal from the control mechanism (E), and a measuring apparatus for the liquid absorption amount of a solid sample is disclosed. (Refer to Patent Document 2 "Configuration".)

[0006]

Table 1

[0007] Next, Patent Document 3 discloses an analysis method of a sample, which has a measurement step of performing measurement on a mixture obtained by mixing while dropping a liquid onto the sample in the apparatus, a post-treatment step of adding and mixing a solid additive that absorbs the liquid to the sample after the measurement step, and a cleaning step of removing the mixture of the sample and the additive from the apparatus after the post-treatment step.

[0008] However, the prior art described so far has had the following problems. Conventionally, the evaluation process of the absorption amount (oil absorption amount) mainly includes a "measurement process" of measuring the added amount of oil when the sample is mixed while adding oil and thickens as the sample absorbs the oil, and the resistance of the rotating blade (hereinafter also referred to as "torque") reaches the maximum (in some cases, the end point is when it reaches 70% of the maximum torque), and a "removal process (i.e., cleaning process)" of removing the analyzed sample after measurement from the mixing cell (hereinafter also simply referred to as "cell") in order to replace the analyzed sample after measurement with the next sample.

[0009] In the cell during the "removal process", the analyzed sample that has absorbed oil to saturation and thickened is adhered, stuck, or fixed. Even if the operator disassembles the cell and tries to scrape off the analyzed sample adhering to its inner wall and rotating blade with a spatula or the like, it is difficult to remove all of it, and a detailed removal operation using a dedicated cleaning sheet (paper or cloth) is required. Therefore, the time required for evaluating the oil absorption amount is, for example, about 30 minutes per sample when the oil absorption amount of the sample is about 20 ml / 100 g. Although the "measurement process" takes about 10 minutes, the "removal process" takes about 20 minutes, and since the "removal process" takes twice as long as the "measurement process", it is a very inefficient operation.

[0010] On the other hand, first, in the technology of Patent Document 1, although the cleaning of the cell is automatically performed by a fully automatic measuring device and the working efficiency is improved, the slurry adhering to the details and narrow parts of the cell, such as the shaft of the rotating blade, cannot be sufficiently removed. As the number of measurements increases, the amount of residue increases, leading to a decrease in the reliability of the measurement results due to fluctuations in the torque signal, contamination, etc. Moreover, it will also lead to the situation that the shaft of the rotating blade is overloaded and the device stops urgently.

[0011] Also, this technology has the disadvantage that the slurry scatters and contaminates the surroundings in order to blow air on the disassembled cell. In addition to these, in the cell, the solubility parameter (cal / cm 3 L) 1 / 2In order to add a liquid for removal with a difference of 3 or more to 0.5 to 2.0 times (by weight) of the solid sample to form a slurry, there are problems such as an increase in the amount of waste and a high treatment cost, and frequent clogging of pipes when sending the slurry to the waste tank.

[0012] Next, in the technique of Patent Document 2, this technique is originally an improved version of the technique of Patent Document 1. By sucking and removing the slurry in the cell through the suction nozzle for removal, the inconvenience of the slurry splashing and soiling the surroundings is eliminated, but otherwise, it has the same problems as the technique of Patent Document 1.

[0013] Next, in the technique of Patent Document 3, in the removal step, the analyzed sample to which a solid additive for absorbing oil is added is scraped off onto a tray with a spatula while disassembling the cell, and then sucked with a vacuum cleaner. By this operation, most of the analyzed sample can be quickly removed. However, still, the cell has to be disassembled every time one specimen is processed, and for removing the analyzed sample adhering to the axis of the rotating blade and the like in the details and narrow parts of the cell, cleaning with a spatula or a sheet is still essential. The effect of simplifying the labor and shortening the time required for the work is insufficient, and there is still much room for improvement.

Prior Art Documents

Patent Documents

[0014]

Patent Document 1

Patent Document 2

Patent Document 3

Summary of the Invention

Problems to be Solved by the Invention

[0015] Therefore, an object of the present invention is to newly provide a technique that can perform a more efficient, careful, and low-cost removal process while obtaining a correct evaluation result in the evaluation of the absorption amount. More specifically, an object of the present invention is to newly provide a technique that does not perform cell decomposition and cleaning with a spatula or a sheet, has no accumulation of residues, does not contaminate the surroundings, and does not require a large amount of addition of a removal liquid.

Means for Solving the Problems

[0016] As a result of intensive research on the above problems, the present inventor has found that by using an absorbent that absorbs the solvent absorbed by the sample in reverse, not only can the viscosity of the sample be reduced, but also, while injecting a gas such as air into the cell, after sucking the sample from a suction port such as a nozzle with a brush, by flowing the dirt remaining in the cell with a cleaning liquid, it is possible to easily perform the removal work of fine parts and narrow parts without disassembling the cell, and thus the present invention has been completed.

[0017] That is, according to one aspect of the present invention for solving the above problems, a first aspect of the present invention includes a first preparation step of putting a sample into a mixing container equipped with a stirring part, a measurement step of measuring the value of the resistance generated between the first mixed sample in the mixing container obtained by mixing while adding a first solvent to the sample and the stirring part during the mixing, an evaluation step of obtaining the absorption amount of the sample from the value of the resistance, a second preparation step of putting a solvent absorbent into the first mixed sample in the mixing container, a reaction step of mixing the first mixed sample and the solvent absorbent to obtain a second mixed sample, a removal step of removing the second mixed sample from the mixing container by sucking while injecting a gas to crush the second mixed sample, and a cleaning step of cleaning the mixing container by sucking while injecting a second solvent into the mixing container after the removal step. The absorption amount evaluation method is characterized by having these steps.

[0018] A second aspect of the present invention is an absorption amount evaluation method characterized in that the stirring part in the first aspect includes a rotor and a rotating shaft.

[0019] The third aspect of the present invention is a method for evaluating the absorption amount, characterized in that the sample in the first aspect is a powder.

[0020] The fourth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the first solvent in the first aspect contains one or more selected from dibutyl phthalate (DBP), N-methyl-2-pyrrolidone (NMP), and water.

[0021] The fifth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the solvent absorbent in the first aspect is a substance of the same kind as the sample and / or a substance having an absorption amount of 10 ml / 100 g or more.

[0022] The sixth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the solvent absorbent in the first aspect is a substance having an absorption amount of 14 ml / 100 g or more.

[0023] The seventh aspect of the present invention is a method for evaluating the absorption amount, characterized in that the addition amount of the solvent absorbent in the first aspect is less than 0.5 times (weight times) of the sample.

[0024] The eighth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the gas in the first aspect is air.

[0025] The ninth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the suction in the first aspect is performed by a vacuum cleaner.

[0026] The tenth aspect of the present invention is a method for evaluating the absorption amount, characterized in that the second solvent in the first aspect contains ethanol.

[0027] The eleventh aspect of the present invention is an absorption amount evaluation system, characterized by having at least an absorption amount measuring device, an injection device, and a suction device.

[0028] The twelfth aspect of the present invention is an absorption amount evaluation system characterized in that the injection device in the eleventh aspect is an air gun and the suction device is a vacuum cleaner.

Advantages of the Invention

[0029] According to the present invention, in the evaluation of the absorption amount, it is possible to newly provide a technique that can perform the removal process more efficiently, carefully, and at low cost while obtaining a correct evaluation result. More specifically, it is possible to newly provide a technique that does not perform the decomposition of cells and cleaning with a spatula or a sheet, has no accumulation of residues, does not stain the surroundings, and does not require the addition of a large amount of removal liquid, and has a remarkable industrial effect.

Brief Description of the Drawings

[0030]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Embodiments for Carrying Out the Invention

[0031] Hereinafter, specific embodiments of the present invention will be described in detail with reference to the drawings and the like. The present invention is not limited to the following embodiments, and can be appropriately modified without changing the gist of the present invention. In each drawing, part or all of them are schematically described, and the scale is changed. Further, in this specification, "~" refers to a value equal to or more than a predetermined value and equal to or less than a predetermined value, and "●, and / or, ▲" means "either ● or ▲, or both".

[0032] Figure 1 is an operation flowchart showing an overall view of the absorption amount evaluation method according to the present invention. Specific embodiments of the present invention will be described below in the following order with reference to this Figure 1. 1. Absorption amount evaluation method 1-1. First preparation step 1-2. Measurement step 1-3. Evaluation step 1-4. Second preparation step 1-5. Reaction step 1-6. Removal step 1-7. Washing step 2. Effects in the embodiment

[0033] 1. Absorption amount evaluation method The evaluation method used in the present invention is not particularly limited. As a specific example, an evaluation method is shown below in which a first solvent is added to a sample in a mixing container while mixing, and the value of the resistance generated between the obtained first mixed sample in the mixing container and the stirring unit during the mixing is measured.

[0034] 1-1. First preparation step In the step of charging a sample into a mixing container, the mixing container to be used is provided with a stirring unit. The stirring form of this stirring unit is not limited to only a rotating blade. For example, it may be a stirring blade having a plurality of blades like a windmill, and the number thereof is not limited either. Further, the mixing container is not limited to only a mixing cell. For example, a structure in which the container itself rotates like a concrete mixer truck may be used, and all containers used for mixing samples correspond to this. Furthermore, the sample to be evaluated is not particularly limited as long as it absorbs the first solvent. For example, in addition to powders such as carbon powder, pigment powder, and metal compound powder, aggregates formed by aggregation of powders may also be used. In the present invention, it is preferable that the stirring unit includes a rotary blade and a rotating shaft, the mixing container is a mixing cell, and the sample is a powder. Further, the rotation speed of the rotary blade is preferably 100 to 300 rpm, and the sample amount is preferably 20 to 200 g.

[0035] 1-2. Measurement step This is a step of measuring the value of the resistance generated between the obtained first mixed sample in the mixing container and the stirring unit during the mixing while adding the first solvent to the sample. When a certain amount of sample is put into the mixing container and the rotary blade is operated while adding the first solvent, the mixing progresses over time, a first mixed sample with high viscosity is obtained, and resistance occurs in the rotary blade. Then, when the end point of the measurement is reached, the resistance rapidly increases with respect to the increase in the first solvent, and a curve that decreases after passing through the maximum value of the resistance is drawn as the measurement result. Figure 2 shows the measurement result.

[0036] The first solvent to be used is not particularly limited as long as it can make the sample into a first mixed sample with high viscosity when absorbed by the sample. For example, when the sample is carbon powder, oil or other solvents may be used as the first solvent. In the present invention, it is preferable that the first solvent contains one or more selected from dibutyl phthalate (DBP), N-methyl-2-pyrrolidone (NMP), and water. The addition rate of the first solvent is preferably 1 to 5 ml / min.

[0037] Incidentally, in the measurement process of the prior art, aspects that pose problems in the present invention can be observed as disclosed in FIGS. 3 and 4. FIG. 3 is a reference diagram (photograph) showing an example of an analyzed sample 100 in the prior art, that is, "a mixture (kneaded product) after measurement (Patent Documents 1 and 2)", "a sample after the measurement process (Patent Document 3)". This "mixture (kneaded product) after measurement" and "sample after the measurement process" correspond to the "first mixed sample" according to the present invention. FIG. 4 is a reference diagram (photograph) showing an example of the operation of disassembling the mixing container and removing the analyzed sample 100 in the prior art, that is, "the mixture (kneaded product) after measurement" and "the sample after the measurement process" from the mixing container with a spatula 101. It can be observed that a highly viscous sample adheres to the inner wall of the mixing container, the rotating blades, etc., and the removal work is quite time-consuming.

[0038] 1-3. Evaluation Step This is a step of obtaining the absorption amount of the sample from the resistance value. A load cell (load transducer), which is a sensor for detecting torque, converts torque into an electrical signal. For example, a "strain gauge type transducer", which is a type of load cell, receives the torque generated on the rotating blade with an elastic body, converts the generated "strain" into an electrical quantity, and transmits it to a torque meter. Based on the amount of the first solvent added at the maximum torque, the absorption amount of the sample is calculated. Also, in the present invention, the absorption amount of the sample is preferably determined with the end point within the range of 70 to 100% of the maximum torque, and the unit is preferably expressed as "ml / 100 g", which is the amount of the first solvent added per 100 g of the sample.

[0039] 1-4. Second Preparation Step This is a step of introducing a solvent absorbent (hereinafter also simply referred to as "absorbent") into the mixing container. The solvent absorbent is not particularly limited as long as it can absorb the first solvent contained in the first mixed sample. However, in the case where the sample is the same substance as the sample, for example, when the sample is carbon powder and the first solvent is oil, it is preferable to use the remaining carbon powder as the solvent absorbent. Here, "the same kind" refers to not only the sample itself, but also those whose composition and structure are exactly the same as the sample (for example, those that differ only in the production date from the sample), those that have the same constituent elements as the sample but different composition ratios, and so on. As a result, in the above case, only carbon powder and oil will exist in the mixing container, and the possibility that the mixing of other substances will have an adverse effect on the measurement results can be further reduced. Moreover, since it is not necessary to purchase another solvent absorbent, the cost required for a series of operations in the evaluation can also be reduced.

[0040] Of course, a substance different from the sample may be used as the solvent absorbent. When the absolute amount of the sample is limited, for example, in addition to development products, test and research products that are not mass-produced products, precious metal powders, rare metal powders, etc., it is more advantageous in terms of cost to use something different from the sample as the solvent absorbent rather than the remaining sample. As an example, when the sample is carbon powder or metal compound powder, powders of relatively inexpensive industrial raw materials such as radiolite powder can be used instead of the remaining sample. As a result, the solvent absorbent absorbs the first solvent contained in the first mixed sample, reduces the viscosity of the first mixed sample, and facilitates the removal operation. In addition to the initial effect, the cost required for a series of evaluations can also be reduced. In addition to radiolite powder, calcium carbonate powder, wollanoslite powder, etc. used in wall materials, floor materials, and paints can also be cited as candidates for the solvent absorbent.

[0041] Also, the solvent absorbent preferably has an absorption amount of 10 ml / 100 g or more. If a solvent absorbent with a larger absorption amount than the sample to be evaluated is selected, a smaller input amount is required and the first solvent can be effectively absorbed. However, even if the absorption amount is smaller than that of the sample, as long as the input amount is increased, the first solvent contained in the first mixed sample can be sufficiently absorbed. However, in terms of reducing the amount of waste and the treatment cost, it is preferable that the solvent absorbent has an absorption amount of 14 ml / 100 g or more, more preferably 17 ml / 100 g or more, and particularly preferably 20 ml / 100 g or more. By using a substance with an absorption amount of 14 ml / 100 g or more, the addition amount can be less than 0.5 times (weight ratio) of the sample, and it is not necessary to add the liquid for removal as in Patent Documents 1 and 2 in an amount of 0.5 to 2.0 times (weight ratio) of the solid sample.

[0042] Thus, the input amount of the solvent absorbent is not particularly limited, but it is preferable to confirm the optimal input amount in advance according to the combination of the sample, the first solvent, and the solvent absorbent. As a confirmation method, for example, after a preliminary measurement of the sample, the solvent absorbent is gradually added step by step to the mixing container and stirred together with the first mixed sample repeatedly. Then, when gas is injected onto the first mixed sample adhering to the inner wall of the mixing container or the rotor blade, if it can be easily peeled off, that amount can be set as the optimal input amount.

[0043] 1 - 5. Reaction step This is a step of mixing the first mixed sample and the solvent absorbent to react with each other, that is, absorbing the first solvent contained in the first mixed sample by the solvent absorbent to obtain a second mixed sample with a lower viscosity than the first mixed sample.

[0044] The mixing time of the first mixed sample and the solvent absorbent is not particularly limited, but in order to obtain the second mixed sample while ensuring that the first solvent contained in the first mixed sample is surely absorbed by the solvent absorbent and the overall time spent on evaluation does not become long, it is preferably 0.5 to 2 minutes. Also, the rotation speed of the rotor blade is preferably 100 to 300 rpm. In this reaction step, it is visually confirmed that the first mixed sample, which was in a high-viscosity state (for example, a starch-like state) with the solvent absorbent having absorbed the first solvent, has returned to a low-viscosity state (for example, a flake-like state) as the second mixed sample. However, in addition to this, the state (feel) of the second mixed sample can also be confirmed at the tip of a rod-shaped jig or the like.

[0045] 1 - 6. Removal step A step of aspirating while injecting a gas into the second mixed sample to remove the second mixed sample from the mixing container.

[0046] In the prior art, that is, in Patent Document 3, the mixing container has to be disassembled every time one sample is processed. Also, for removing analyzed samples and the like clogged in the gaps between the rotating blades and the rotating shaft, and for removing debris from the detailed and narrow parts of the mixing container, cleaning with a spatula or a sheet is essential. In contrast, in this removal step, without disassembling the mixing container and without performing removal work with a spatula or a sheet, while injecting a gas such as air into the second mixed sample in the mixing container, particularly the second mixed sample adhering to the detailed and narrow parts of the mixing container (while blowing or ejecting the second mixed sample), the second mixed sample is aspirated from a suction port such as a nozzle with a brush. By doing so, accumulation of residues as in Patent Documents 1 and 2 is eliminated, and the inconvenience of slurry scattering and soiling the surroundings as in Patent Document 1 is also resolved.

[0047] FIG. 5 is a schematic diagram showing an example of the “removal step” in the absorption amount evaluation method according to the present invention. In FIG. 5, 1 is the main part of the mixing container, 2 is the rotating blade, 3 is the mixing container fixing hole, 4 is the gas injection device, 5 is the suction port, 6 is the second mixed sample, 7 represents the injection direction, and 8 represents the suction direction. The gas used for injection is not limited to only air, and may be selected from non - oxygen - containing gases such as carbon dioxide, as well as inert gases such as nitrogen, argon, and helium, and mixtures of these gases. However, it is preferable to use air.

[0048] The injection device 4 used for injection is not particularly limited. For example, it includes a gun - type device in which gas is injected by pulling a trigger, or a penlight - type device in which gas is injected by pressing a button or a switch. Also, an air duster used when cleaning a computer keyboard, etc., can also be cited as one of the options. The suction port 5 used for suction is not particularly limited, but a nozzle with a brush or the like that can sweep up the second mixed sample adhering to the detailed and narrow parts of the mixing container during suction is preferably used. The suction device (not shown) used for suction through the suction port 5 is not particularly limited, but a wet / dry vacuum cleaner or the like that can also handle the organic solvent itself (i.e., the second solvent used in the subsequent cleaning step) and substances containing the organic solvent (i.e., the second mixed sample) is preferably used.

[0049] 1-7. Cleaning Step This is a step of cleaning the mixing container by sucking while injecting the second solvent into the mixing container after the removal step. The dirt derived from the second mixed sample adhering to the inner wall of the mixing container, the rotating blade, etc. is washed away by spraying the second solvent (before cleaning), and the second solvent (after cleaning) is sucked. FIG. 6 is a schematic diagram showing an example of the "cleaning step" in the absorption amount evaluation method according to the present invention. In FIG. 6, reference numeral 1 is the main part of the mixing container, 2 is the rotating blade, 3 is the mixing container fixing hole, 5 is the suction port, 7 is the injection direction, 8 is the suction direction, 9 is the second solvent (before cleaning) injector, and 10 is the second solvent (after cleaning).

[0050] Examples of the second solvent include ethanol, normal propyl alcohol (NPA), dodecane, hexadecane, cyclohexane, glycerin, ethylene glycol, normal butylamine, methyl normal pentyl ketone, diethyl phthalate, water, and mixed organic solvents such as Solmix AP-7 (manufactured by Nippon Alcohol Sales Co., Ltd., registered trademark) and Solmix HP-7 (manufactured by Nippon Alcohol Sales Co., Ltd., registered trademark). Among these, it is preferable to use ethanol, normal propyl alcohol, Solmix AP-7 (manufactured by Nippon Alcohol Sales Co., Ltd., registered trademark), and Solmix HP-7 (manufactured by Nippon Alcohol Sales Co., Ltd., registered trademark). Also, these second solvents may be used alone, one selected from the above second solvents, or two or more may be mixed and used.

[0051] The injection device 9 (the second solvent (before cleaning) injector) used for injection is not particularly limited. For example, it can be a washing bottle type that is most commonly used in the widest range of fields, or a gun type that is used for spraying cleaning agents for window cleaning and bathtub cleaning, or disinfectant liquids for clothes and shoes. Regarding the suction port 5 used for suction and the suction device (not shown) used for suction via the suction port 5, it is the same as the description in the removal step of the previous process.

[0052] Also, when the second solvent is difficult to dry, a drying operation using a dryer or the like may be appropriately performed. By doing so, the inside of the mixing container can be kept in a better state than when cleaning with a spatula or a sheet as in Patent Document 3.

[0053] 2. Effects in the Embodiment According to the present embodiment, all the problems in Patent Documents 1 to 3 can be improved. That is, the inconvenience of the slurry splashing and soiling the surroundings as in Patent Document 1 is eliminated, the accumulation of residues as in Patent Documents 1 and 2 is eliminated, and the second mixed sample in the mixing container can be extremely easily removed without disassembling the mixing container and performing removal operations with a spatula or a sheet as in Patent Document 3. Thereby, the surrounding environment can be kept clean, the reliability of measurement results due to contamination and the like can be prevented from decreasing, the load on the measuring device can be reduced, and further, the labor and time required for the work can be simplified, and the effect of shortening the time can be sufficiently obtained, and the number of samples that can be processed in a day can be increased, and the work efficiency is remarkably improved.

[0054] In addition, the present embodiment not only relates to the evaluation work, but also exhibits the same effects when adopted as a post-treatment step (i.e., cleaning step) when manufacturing a mixture, and the manufacturing process related to the mixture can be efficiently repeated a plurality of times. It goes without saying that the present embodiment can be applied even when using carbon black or the like in the tire manufacturing industry as a sample. In addition, it can also be applied in the fields of metal smelting and civil engineering building materials. However, the application range of the present embodiment is not limited to these.

Example

[0055] Hereinafter, the present invention will be specifically described using Examples and Comparative Examples. However, the present invention is not limited in any way by the following Examples and Comparative Examples. For the absorption amount measuring device used, the absorption amount measuring instrument S-500 (manufactured by Asahi Riken Co., Ltd.) was used. For injecting gas into the second mixed sample, the air gun HBA (manufactured by AS ONE Corporation), which is a gun-type gas injection device 4, was used. And for sucking the second mixed sample and the second solvent after washing, a JET Pearl can cleaner (manufactured by Sankei Kiki Co., Ltd.), which is a vacuum cleaner, with a suction port 5 to which a vacuum cleaner nozzle (with brush) (manufactured by DAISO Co., Ltd.) was attached was used. With this configuration, an absorption amount evaluation system according to the present invention was constructed. Furthermore, by installing each of the above devices in a standard draft chamber DC-150 (manufactured by Aspec Kogyou Co., Ltd.), which is a local exhaust device, measures were taken against the working environment such as dust, organic solvent mist, and odor.

Example

[0056] For the sample, Compound A (powder) was used. For the solvent absorbent, an amount corresponding to the remaining amount of Compound A (powder) was used. For the first solvent, dibutyl phthalate (DBP) was used, and for the second solvent, ethanol was used. First, 100 g of the sample was put into a mixing container (mixing cell), and the measurement in auto mode was started with the addition rate of the first solvent being 2 ml / min and the rotation speed of the rotor being 200 rpm.

[0057] After the automatic mixing (measurement) time of 10 to 15 minutes elapsed and the measurement was completed to obtain the measurement result (ml / 100 g) of the absorption amount (oil absorption amount), 20 g of the solvent absorbent was added to the generated first mixed sample, and manual mixing was performed for 1 minute in manual mode with the rotation speed of the rotor being 200 rpm. Next, it was visually confirmed that the first mixed sample, in which the solvent absorbent had absorbed all of the first solvent and had become in a high-viscosity state (paste-like), had returned to a low-viscosity state (flake-like) as the second mixed sample.

[0058] Next, without disassembling the mixing container, while appropriately changing the angle of the rotor, the second mixed sample was removed by suction while injecting air from all directions. Next, while appropriately changing the angle of the rotor, the inside of the mixing container was washed by suction while injecting the second solvent from all directions using a wash bottle.

[0059] The above operation was repeated 10 times, and 10 measurement results of the absorption amount (oil absorption amount) were obtained. Details such as the evaluation conditions and evaluation results at this time are shown in Tables 2 and 3.

Example

[0060] The same operation as in Example 1 was performed except that radiolite (5 g) was used as the solvent absorbent.

[0061] (Comparative Example 1) After obtaining the measurement result of the absorption amount (oil absorption amount), 50 g of water was added as the removal liquid instead of the solvent absorbent, and manual mixing was performed in manual mode. Next, after installing a plastic tray under the kneading chamber (corresponding to the "mixing container" according to the present invention), the kneading chamber was disassembled, and compressed air was supplied from above to remove the mixture after the measurement was completed and to dry the kneading chamber. Next, the kneading chamber was assembled without performing the washing operation with the second solvent. The same operation as in Example 1 was performed except for the above operation, and an attempt was made to simulate the technique described in Patent Document 1.

[0062] (Comparative Example 2) After obtaining the measurement result of the absorption amount (oil absorption amount), 50 g of water was added as the removal liquid instead of the solvent absorbent, and manual mixing was performed in manual mode. Next, without disassembling the kneading chamber, after sucking and removing the slurry in the kneading chamber through the suction nozzle for removal from above (in a state where the "nozzle with brush" according to the present invention is removed), compressed air was supplied from above (not applied to wipe off and remove the slurry in the kneading chamber as described in Patent Document 2, but used to dry the inside of the kneading chamber), and the kneading chamber was dried. Also, the cleaning operation with the second solvent was not performed. Except for the above operations, the same operations as in Example 1 were performed, and an attempt was made to simulate the technique described in Patent Document 2.

[0063] (Comparative Example 3) After visually confirming that the sample after the measurement step (corresponding to the "first mixed sample" according to the present invention) was in the state of a mixture of the sample after the post-treatment step and the additive (corresponding to the "second mixed sample" according to the present invention), a plastic tray was placed under the mixing cell (corresponding to the "mixing container" according to the present invention), the mixing cell was disassembled, and while dropping the mixture of the sample after the post-treatment step and the additive onto the tray, cleaning was performed with a spatula or a sheet. Next, the mixture of the sample after the post-treatment step and the additive dropped onto the tray was sucked. Also, the cleaning operation with the second solvent was not performed. Except for the above operations, the same operations as in Example 1 were performed, and an attempt was made to simulate the technique described in Patent Document 3.

[0064]

Table 2

[0065]

Table 3

[0066] [General Evaluation] In Examples 1 and 2 within the scope of the present invention, even though the cells were not disassembled and the cleaning with a spatula or a sheet was not performed, there was no accumulation of residues, the surroundings were not soiled, the amount of waste was small, the working time was short, and furthermore, it was found that the evaluation results of the absorption amount (oil absorption amount) also had little variation and more accurate values were obtained.

[0067] On the other hand, in Comparative Examples 1 to 3 that deviated from the scope of the present invention and attempted to simulate the prior art (Patent Documents 1 to 3), in all aspects such as being affected by the accumulation of residues and the evaluation results being biased high, effects comparable to those of the present invention were not obtained. That is, according to the present invention, in the evaluation of the absorption amount, while obtaining correct evaluation results, the removal process can be carried out more efficiently, carefully, and at low cost without disassembling the cells and cleaning with a spatula or a sheet, without accumulation of residues, without soiling the surroundings, and without the need for a large amount of addition of the removal liquid. It is clear that a new technology can be provided, and the above results are sufficient to support this.

[0068] The technical scope of the present invention is not limited to the aspects described in the above-mentioned embodiment. One or more of the requirements described in the above-mentioned embodiment may be omitted. In addition, the requirements described in the above-mentioned embodiment can be combined as appropriate. Furthermore, as long as permitted by law, the contents of all the documents cited in this specification are incorporated and made part of the description of the text.

Explanation of Reference Numerals

[0069] 1 Main part of the mixing container 2 Rotating blade 3 Fixing hole of the mixing container 4 Gas injection device 5 Suction port 6 Second mixed sample 7 Injection direction 8 Suction direction 9 Injector for the second solvent (before cleaning) 10 Second solvent (after cleaning) 100 Analyzed sample 101 spatula

Claims

1. A first preparation step of introducing a sample into a mixing container equipped with a stirring unit; A measurement step of measuring the value of the resistance generated between the first mixed sample in the mixing container obtained by mixing while adding a first solvent to the sample and the stirring unit during the mixing; An evaluation step of obtaining the absorption amount of the sample from the value of the resistance; A second preparation step of introducing a solvent absorbent into the first mixed sample in the mixing container; A reaction step of mixing the first mixed sample and the solvent absorbent to obtain a second mixed sample; A removal step of removing the second mixed sample from the mixing container by sucking while crushing by injecting a gas into the second mixed sample; A cleaning step of cleaning the mixing container by sucking while injecting a second solvent into the mixing container after the removal step; An absorption amount evaluation method characterized by comprising the above.

2. The absorption amount evaluation method according to claim 1, characterized in that the stirring unit includes a rotating blade and a rotating shaft.

3. The absorption amount evaluation method according to claim 1, characterized in that the sample is a powder.

4. The absorption amount evaluation method according to claim 1, characterized in that the first solvent contains one or more selected from di-n-butyl phthalate (DBP), N-methyl-2-pyrrolidone (NMP), and water.

5. The absorption amount evaluation method according to claim 1, characterized in that the solvent absorbent is a substance of the same kind as the sample and / or a substance having an absorption amount of 10 ml / 100 g or more.

6. The absorption amount evaluation method according to claim 1, characterized in that the solvent absorbent is a substance having an absorption amount of 14 ml / 100 g or more.

7. The absorption amount evaluation method according to claim 1, characterized in that the addition amount of the solvent absorbent is less than 0.5 times (weight times) that of the sample.

8. The absorption amount evaluation method according to claim 1, characterized in that the gas is air.

9. The absorption amount evaluation method according to claim 1, characterized in that the suction is performed by a vacuum cleaner.

10. The absorption amount evaluation method according to claim 1, characterized in that the second solvent contains ethanol.

11. An absorption amount evaluation system characterized by having at least an absorption amount measuring device, an injection device, and a suction device.

12. The injection device is an air gun, The absorption amount evaluation system according to claim 11, characterized in that the suction device is a vacuum cleaner.

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