JP7433574B2 - Viscosity measuring device - Google Patents

Viscosity measuring device Download PDF

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JP7433574B2
JP7433574B2 JP2020137588A JP2020137588A JP7433574B2 JP 7433574 B2 JP7433574 B2 JP 7433574B2 JP 2020137588 A JP2020137588 A JP 2020137588A JP 2020137588 A JP2020137588 A JP 2020137588A JP 7433574 B2 JP7433574 B2 JP 7433574B2
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solvent
slurry
viscosity
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storage container
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JP2022033602A (en
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康爾 堺
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JFE Steel Corp
Kobe Steel Ltd
Nippon Steel Corp
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JFE Steel Corp
Kobe Steel Ltd
Nippon Steel Corp
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Description

本発明は、粘度測定装置に関する。 The present invention relates to a viscosity measuring device.

無灰炭の製造方法として、石炭と溶剤とを混合したペースト状混合物を加熱することにより石炭中の可溶成分を溶剤中に溶出させる工程と、固液分離により可溶成分が溶け込んだ溶液を取り出す工程と、この溶液から溶剤を蒸発させることで石炭の可溶成分のみを取り出す工程とを含む製造方法が知られている。 The method for producing ash-free coal involves two steps: heating a pasty mixture of coal and a solvent to elute the soluble components in the coal into the solvent, and separating the soluble components into a solution using solid-liquid separation. A manufacturing method is known that includes a step of taking out the coal and a step of taking out only the soluble components of the coal by evaporating the solvent from the solution.

前記可溶成分を取り出す工程では、複数の分離器を用いて前記溶剤を蒸発させることがある。一の分離器を用いて前記溶液から前記溶剤を蒸発させて無灰炭及び前記溶剤を含むペースト状混合物とし、このペースト状混合物を他の分離器に移送する際のハンドリングは、前記ペースト状混合物の粘度によっては困難になることがある。また、前記分離器等のペースト状混合物を用いる機器の開発においても前記ペースト状混合物の粘度を考慮する必要がある。前記ペースト状混合物の粘度は、前記ペースト状混合物の溶剤含有率の影響を受けるため、ペースト状混合物の溶剤含有率と粘度との関係を容易に把握できる方法が望まれている。 In the step of taking out the soluble components, the solvent may be evaporated using a plurality of separators. The solvent is evaporated from the solution using one separator to form a paste mixture containing ash-free charcoal and the solvent, and the handling when transferring this paste mixture to another separator is as follows: This may be difficult depending on the viscosity of the Furthermore, in the development of equipment such as the separator that uses a pasty mixture, it is necessary to consider the viscosity of the pasty mixture. Since the viscosity of the pasty mixture is affected by the solvent content of the pasty mixture, there is a need for a method that can easily determine the relationship between the solvent content and viscosity of the pasty mixture.

タール誘導品、タール、又はピッチ等の流体物の粘度を自動的に測定する粘度測定システムが発案されている（特開平６－１０９６１４号公報）。この粘度測定システムは、温度管理されたサンプルを設定された回転速度でロータが粘性抵抗に基づいて粘度の測定を行うため、測定作業の効率化及び迅速化を図ることができ、測定コストを低減することができるとされている。 A viscosity measuring system for automatically measuring the viscosity of fluids such as tar derivatives, tar, or pitch has been proposed (Japanese Patent Laid-Open No. 6-109614). This viscosity measurement system uses a rotor to measure the viscosity of a temperature-controlled sample at a set rotation speed based on viscous resistance, making measurement work more efficient and faster, and reducing measurement costs. It is said that it can be done.

特開平６－１０９６１４号公報Japanese Patent Application Publication No. 6-109614

上記公報所載の粘度測定システムでは、所定の温度にしたサンプルの粘度を測定するため、前記サンプルの温度と粘度との関係を把握することはできるが、前記サンプル中の液体の含有量が測定できるものではないため、前記サンプルの液体含有率と粘度との関係を把握することは容易にできないおそれがある。 The viscosity measurement system described in the above publication measures the viscosity of a sample heated to a predetermined temperature, so it is possible to understand the relationship between the temperature and viscosity of the sample, but the liquid content in the sample cannot be measured. Therefore, it may not be possible to easily understand the relationship between the liquid content and viscosity of the sample.

上述のような事情に鑑みて、本発明は、溶剤を含むスラリーの溶剤含有率と粘度との関係を容易に把握することができる粘度測定装置を提供することを課題とする。 In view of the above-mentioned circumstances, an object of the present invention is to provide a viscosity measuring device that can easily determine the relationship between the solvent content and viscosity of a slurry containing a solvent.

前記課題を解決するためになされた本発明の一態様は、溶剤を含むスラリーの粘度測定装置であって、前記スラリーの粘度を測定する粘度測定部と、前記粘度測定部で測定される前記スラリーを加温する加温部と、前記加温により蒸発した前記溶剤を回収する溶剤回収部と、前記溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出する算出部とを備える粘度測定装置である。 One aspect of the present invention made to solve the above problem is a viscosity measuring device for a slurry containing a solvent, which includes a viscosity measuring section that measures the viscosity of the slurry, and a viscosity measuring section that measures the viscosity of the slurry. A viscosity measuring device comprising: a heating unit that heats the slurry; a solvent recovery unit that recovers the solvent evaporated by the heating; and a calculation unit that calculates the solvent content in the slurry from the amount of evaporation of the solvent. .

当該粘度測定装置は、加温部で前記スラリーを加温しつつ、粘度測定部でスラリーの粘度を測定するため、溶剤の蒸発量が変化したスラリーにおける粘度を測定することができる。また、溶剤回収部で蒸発した前記溶剤を回収し、算出部で前記回収した溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出することができる。このように、溶剤が蒸発した前記スラリーにおける前記溶剤含有率と前記粘度とを測定することができるため、前記スラリーにおける前記溶剤含有率と前記粘度との関係を把握することが容易にできる。 The viscosity measuring device measures the viscosity of the slurry in the viscosity measuring part while heating the slurry in the heating part, so it is possible to measure the viscosity of the slurry in which the amount of evaporation of the solvent has changed. Further, the evaporated solvent can be recovered in a solvent recovery section, and the solvent content in the slurry can be calculated from the evaporation amount of the recovered solvent in a calculation section. In this way, since the solvent content and the viscosity in the slurry from which the solvent has evaporated can be measured, it is easy to understand the relationship between the solvent content and the viscosity in the slurry.

前記溶剤回収部が、前記蒸発した溶剤を液化する凝縮機構を有することが好ましい。液体を測定することは比較的容易であるため、前記蒸発した溶剤を液化し、この液化された溶剤を測定して算出することで前記スラリーから蒸発した溶剤の蒸発量を容易に知得することができる。 It is preferable that the solvent recovery section has a condensation mechanism that liquefies the evaporated solvent. Since it is relatively easy to measure a liquid, it is possible to easily determine the amount of solvent evaporated from the slurry by liquefying the evaporated solvent and measuring and calculating the liquefied solvent. can.

前記溶剤回収部が、前記凝縮機構で液化された溶剤の重量を測定する重量測定機構をさらに有することが好ましい。液化した前記溶剤の体積を測定してもよいが、比較的容易に測定できる前記溶剤の重量から前記蒸発量を算出するとよい。重量測定機構を有することで前記液化した溶剤の重量を容易に測定することができ、前記蒸発量をより容易に知得することができる。 Preferably, the solvent recovery section further includes a weight measuring mechanism that measures the weight of the solvent liquefied by the condensing mechanism. Although the volume of the liquefied solvent may be measured, it is preferable to calculate the evaporation amount from the weight of the solvent, which can be measured relatively easily. By having a weight measurement mechanism, the weight of the liquefied solvent can be easily measured, and the amount of evaporation can be more easily determined.

前記溶剤含有率が所定の閾値以下でスラリーを前記粘度測定部に追加するスラリー供給部をさらに備えることが好ましい。前記溶剤の蒸発量が増大すると前記スラリーの体積が減少して前記粘度測定部における粘度測定が困難になるおそれがある。前記スラリー供給部を備えることで常に所定量以上のスラリーが前記粘度測定部に存在するため、安定して粘度測定をすることができる。 It is preferable to further include a slurry supply section that adds slurry to the viscosity measuring section when the solvent content is below a predetermined threshold value. If the amount of evaporation of the solvent increases, the volume of the slurry may decrease, making it difficult to measure the viscosity in the viscosity measuring section. By providing the slurry supply section, a predetermined amount or more of slurry is always present in the viscosity measuring section, so that viscosity can be measured stably.

上述のように、本発明の粘度測定装置は、溶剤を含むスラリーの溶剤含有率と粘度との関係を容易に把握することができる。 As described above, the viscosity measuring device of the present invention can easily determine the relationship between the solvent content and viscosity of a slurry containing a solvent.

図１は、本発明の一実施形態に係る粘度測定装置の構成を示す模式的平面図である。FIG. 1 is a schematic plan view showing the configuration of a viscosity measuring device according to an embodiment of the present invention. 図２は、無灰炭と溶剤とを含むスラリーの溶剤含有率及び粘度の経時変化を示すグラフである。FIG. 2 is a graph showing changes over time in the solvent content and viscosity of a slurry containing ash-free charcoal and a solvent. 図３は、図２のスラリーの溶剤含有率と粘度との関係を示すグラフである。FIG. 3 is a graph showing the relationship between the solvent content and viscosity of the slurry shown in FIG.

以下、適宜図面を参照しつつ、本発明の実施の形態を詳説する。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings as appropriate.

図１に、本発明の一実施形態である粘度測定装置１の構成を示す。 FIG. 1 shows the configuration of a viscosity measuring device 1 that is an embodiment of the present invention.

［粘度測定装置］
当該粘度測定装置１は、スラリーの粘度を測定する粘度測定部２と、粘度測定部２で測定される前記スラリーを加温する加温部３と、加温により蒸発した溶剤を回収する溶剤回収部４と、前記溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出する算出部（不図示）とを備える。 [Viscosity measuring device]
The viscosity measuring device 1 includes a viscosity measuring section 2 for measuring the viscosity of slurry, a heating section 3 for heating the slurry measured by the viscosity measuring section 2, and a solvent recovery section for recovering the solvent evaporated by heating. 4, and a calculation section (not shown) that calculates the solvent content in the slurry from the evaporation amount of the solvent.

〔粘度測定部〕
粘度測定部２は、スラリーの粘度を測定する。粘度測定部２は、前記スラリーを貯留するスラリー貯留容器２１と、このスラリー貯留容器２１に供給された前記スラリーを撹拌する撹拌機２２とを含む。 [Viscosity measurement section]
The viscosity measuring section 2 measures the viscosity of the slurry. The viscosity measurement unit 2 includes a slurry storage container 21 that stores the slurry, and a stirrer 22 that stirs the slurry supplied to the slurry storage container 21.

スラリー貯留容器２１は、その内部において、撹拌機２２の一部が配置され、底部でスラリーを貯留する。スラリー貯留容器２１は、その内部が気密になるように形成されている。スラリー貯留容器２１は、有底筒状のスラリー貯留容器本体２１ａと、天部となるスラリー貯留容器蓋２１ｂとを含む。スラリー貯留容器本体２１ａの外面は、少なくとも一部が後述する加温部３に接している。スラリー貯留容器蓋２１ｂは、スラリーを供給するスラリー供給管Ｐ１、及びスラリーから蒸発した溶剤を排出する溶剤排出管Ｐ２と接続されている。また、スラリー貯留容器蓋２１ｂは、撹拌機２２の一部を内部に導入するための開口部分が形成されている。 A part of the agitator 22 is disposed inside the slurry storage container 21, and the slurry is stored at the bottom. The slurry storage container 21 is formed so that the inside thereof is airtight. The slurry storage container 21 includes a bottomed cylindrical slurry storage container main body 21a and a slurry storage container lid 21b serving as a top portion. At least a portion of the outer surface of the slurry storage container main body 21a is in contact with a heating section 3, which will be described later. The slurry storage container lid 21b is connected to a slurry supply pipe P1 that supplies slurry and a solvent discharge pipe P2 that discharges the solvent evaporated from the slurry. Further, the slurry storage container lid 21b is formed with an opening for introducing a part of the stirrer 22 thereinto.

撹拌機２２は、スラリー貯留容器２１内のスラリーを撹拌し、その粘性抵抗によるトルクを測定する。撹拌機２２は、少なくとも一部が前記スラリーに浸漬され、このスラリーを撹拌する回転ロータと、この回転ロータを先端に有する回転軸と、この回転軸を回転する回転機構と、前記回転軸にかかるトルクを検出するトルク検出器とを有する。この検出されたトルクの値から前記スラリーの粘度を算出することができる。 The stirrer 22 stirs the slurry in the slurry storage container 21 and measures the torque due to its viscous resistance. The stirrer 22 includes a rotating rotor that is at least partially immersed in the slurry and that stirs the slurry, a rotating shaft that has the rotating rotor at its tip, a rotating mechanism that rotates the rotating shaft, and a rotating mechanism that rotates the rotating shaft. It has a torque detector that detects torque. The viscosity of the slurry can be calculated from the detected torque value.

〔加温部〕
加温部３は、スラリーを加温する。具体的には、加温部３は、少なくとも一部の外面が接しているスラリー貯留容器本体２１ａを加温することでスラリー貯留容器２１内の前記スラリーを加温する。スラリー貯留容器本体２１ａの外面の少なくとも一部が加温部３に接するとは、例えば、スラリー貯留容器本体２１ａの一部が加温部３に埋設されている状態である。加温部３としては、特に限定されるものでなく、例えば、電気炉を用いることができる。 [Heating section]
The heating section 3 heats the slurry. Specifically, the heating unit 3 warms the slurry in the slurry storage container 21 by heating the slurry storage container main body 21a with which at least a portion of the outer surface is in contact. At least a portion of the outer surface of the slurry storage container main body 21a is in contact with the heating section 3, for example, when a portion of the slurry storage container main body 21a is buried in the heating section 3. The heating section 3 is not particularly limited, and for example, an electric furnace can be used.

〔溶剤回収部〕
溶剤回収部４は、加温により蒸発した溶剤（以下、「蒸発溶剤」ともいう）を回収する。溶剤回収部４は、回収した溶剤を貯留する溶剤貯留容器４１を含む。具体的には、加温部３で加温された前記スラリーから蒸発した溶剤は、スラリー貯留容器２１と溶剤貯留容器４１とを連通する蒸発溶剤排出管Ｐ２を介して回収される。 [Solvent recovery department]
The solvent recovery section 4 recovers the solvent evaporated by heating (hereinafter also referred to as "evaporated solvent"). The solvent recovery section 4 includes a solvent storage container 41 that stores the recovered solvent. Specifically, the solvent evaporated from the slurry heated in the heating section 3 is recovered via an evaporated solvent discharge pipe P2 that communicates the slurry storage container 21 and the solvent storage container 41.

溶剤貯留容器４１は、その内部が気密になるように形成されている。溶剤貯留容器４１は、有底筒状の溶剤貯留容器本体４１ａと、天部となる溶剤貯留容器蓋４１ｂとを含む。溶剤貯留容器蓋４１ｂは、前記蒸発溶剤を導入するための蒸発溶剤排出管Ｐ２、及び前記蒸発溶剤を排出する溶剤排出管Ｐ３と接続している。 The solvent storage container 41 is formed to be airtight inside. The solvent storage container 41 includes a bottomed cylindrical solvent storage container main body 41a and a solvent storage container lid 41b serving as a top portion. The solvent storage container lid 41b is connected to an evaporative solvent discharge pipe P2 for introducing the evaporated solvent and a solvent discharge pipe P3 for discharging the evaporated solvent.

溶剤回収部４が、前記蒸発溶剤を液化する凝縮機構４２を有するのが好ましい。具体的には、蒸発溶剤排出管Ｐ２の一部が溶剤貯留容器４１と凝縮機構４２とを連通し、蒸発溶剤排出管Ｐ２の残部が凝縮機構４２と溶剤貯留容器４１とを連通するように凝縮機構４２を配設し、この凝縮機構４２が前記蒸発溶剤を冷却して液化し、前記液化された溶剤（以下、「液化溶剤」ともいう）が溶剤貯留容器４１に供給されるのが好ましい。このようにすることで、前記液化溶剤の体積や重量を測定することで前記溶剤の蒸発量を知得することができる。 Preferably, the solvent recovery unit 4 includes a condensation mechanism 42 that liquefies the evaporated solvent. Specifically, a part of the evaporated solvent discharge pipe P2 communicates with the solvent storage container 41 and the condensing mechanism 42, and the remaining part of the evaporated solvent discharge pipe P2 communicates with the condensation mechanism 42 and the solvent storage container 41 for condensation. Preferably, a mechanism 42 is provided, the condensation mechanism 42 cools and liquefies the evaporated solvent, and the liquefied solvent (hereinafter also referred to as "liquefied solvent") is supplied to the solvent storage container 41. By doing so, the amount of evaporation of the liquefied solvent can be determined by measuring the volume and weight of the liquefied solvent.

凝縮機構４２としては、特に限定されるものでなく、例えば、冷媒等により蒸気を冷却して凝縮するコンデンサを用いることができる。 The condensing mechanism 42 is not particularly limited, and for example, a condenser that cools and condenses vapor using a refrigerant or the like can be used.

溶剤回収部４が、前記液化溶剤の重量を測定する重量測定機構４３をさらに有するのが好ましい。このようにすることで、前記液化溶剤の重量を測定し、この測定値から前記蒸発量を算出して前記溶剤の蒸発量を容易に知得することができる。 Preferably, the solvent recovery section 4 further includes a weight measuring mechanism 43 that measures the weight of the liquefied solvent. By doing this, the weight of the liquefied solvent is measured, and the evaporation amount is calculated from the measured value, so that the evaporation amount of the solvent can be easily determined.

溶剤貯留容器４１が重量測定機構４３に載置されることが好ましい。このようにすることで、前記液化溶剤の重量を経時的に測定することができ、前記蒸発量の経時的変化を測定することができる。 Preferably, the solvent storage container 41 is placed on the weight measuring mechanism 43. By doing so, the weight of the liquefied solvent can be measured over time, and the change in the amount of evaporation over time can be measured.

〔算出部〕
算出部は、前記溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出する。具体的には、前記溶剤の蒸発量を算出部に入力して前記スラリーの溶剤含有率を算出する。この算出された溶剤含有率の値と、この溶剤含有率における前記粘性抵抗の値とから前記溶剤含有率と前記スラリーの粘度との関係を把握することができる。 [Calculation part]
The calculation unit calculates the solvent content in the slurry from the evaporation amount of the solvent. Specifically, the amount of evaporation of the solvent is input into a calculation unit to calculate the solvent content of the slurry. The relationship between the solvent content and the viscosity of the slurry can be determined from the calculated solvent content and the viscous resistance value at this solvent content.

溶剤回収部４が、凝縮機構４２を有する場合、前記液化溶剤の体積又は重量、あるいは、体積及び重量を測定し、このような測定値を前記算出部に入力して前記溶剤の蒸発量を算出し、前記スラリーの溶剤含有率をさらに算出すればよい。 When the solvent recovery unit 4 has a condensation mechanism 42, the volume or weight, or the volume and weight, of the liquefied solvent is measured, and such measured values are input to the calculation unit to calculate the evaporation amount of the solvent. However, the solvent content of the slurry may be further calculated.

溶剤回収部４が、重量測定機構４３を有する場合、重量測定機構４３の測定値が前記算出部に電気信号で送信されるように構成し、前記液化溶剤の重量の測定値が前記算出部に自動で入力されるのが好ましい。また、撹拌機２２のトルク検出器の測定値も前記算出部に電気信号で送信されるように構成し、前記スラリーの粘性抵抗によるトルクの測定値が前記算出部に自動で入力されるとよい。前記算出部が、入力された前記液化溶剤の重量と前記スラリーのトルク値とを記憶し、その経時的変化を表、グラフ等にして印刷、表示等できるとよい。このようにすることで、前記スラリーの粘度と前記溶剤含有率との関係を把握することがより容易にできる。 When the solvent recovery section 4 includes a weight measurement mechanism 43, the measurement value of the weight measurement mechanism 43 is configured to be transmitted to the calculation section as an electric signal, and the measurement value of the weight of the liquefied solvent is transmitted to the calculation section. It is preferable that it be entered automatically. Further, it is preferable that the measurement value of the torque detector of the stirrer 22 is also transmitted to the calculation section as an electric signal, and the measurement value of the torque due to the viscous resistance of the slurry is automatically input to the calculation section. . It is preferable that the calculation unit stores the input weight of the liquefied solvent and the torque value of the slurry, and can print or display changes over time in a table, graph, etc. By doing so, it is easier to understand the relationship between the viscosity of the slurry and the solvent content.

〔スラリー供給部〕
当該粘度測定装置１が、溶剤含有率が所定の閾値以下でスラリーを粘度測定部２に追加するスラリー供給部５をさらに備えるのが好ましい。スラリー貯留容器２１内のスラリーを加温して溶剤を蒸発させ続けると前記スラリーの体積が減少し、撹拌機２２の前記回転ロータが少なくとも一部を前記スラリーに浸漬することができなくなるおそれがある。そこで、溶剤含有率が所定の閾値以下になると、すなわち、前記溶剤の蒸発量が所定量以上になるとスラリー供給部５がスラリー貯留容器２１にスラリーを供給し、前記回転ロータが少なくとも一部を前記スラリーに常に浸漬できるようにすることが好ましい。このようにすることで、撹拌機２２が前記スラリーの粘性抵抗からのトルクを安定して検出することができる。 [Slurry supply section]
Preferably, the viscosity measuring device 1 further includes a slurry supply section 5 that adds slurry to the viscosity measuring section 2 when the solvent content is below a predetermined threshold. If the slurry in the slurry storage container 21 continues to be heated to evaporate the solvent, the volume of the slurry will decrease, and there is a possibility that the rotating rotor of the agitator 22 will not be able to immerse at least a portion of the slurry in the slurry. . Therefore, when the solvent content becomes less than a predetermined threshold value, that is, when the evaporation amount of the solvent becomes more than a predetermined amount, the slurry supply section 5 supplies the slurry to the slurry storage container 21, and the rotating rotor supplies at least a part of the slurry to the slurry storage container 21. It is preferable to allow constant immersion in the slurry. By doing so, the stirrer 22 can stably detect the torque due to the viscous resistance of the slurry.

スラリー供給部５が、上記算出部から前記溶剤の蒸発量を電気信号で送信されるように構成し、上記蒸発量があらかじめ設定された閾値以上になるとスラリーを自動で供給するとよい。 It is preferable that the slurry supply section 5 is configured so that the amount of evaporation of the solvent is transmitted from the calculation section as an electric signal, and automatically supplies the slurry when the amount of evaporation exceeds a preset threshold value.

［粘度測定方法］
当該粘度測定装置１による粘度測定方法は、スラリー貯留容器２１内のスラリーを加温部３で加温しつつ撹拌機２２で撹拌し、前記スラリーの粘性抵抗を検出する工程と、前記スラリーから蒸発する溶剤を溶剤回収部４で回収して前記溶剤の蒸発量を測定する工程と、前記蒸発量から前記スラリーにおける溶剤含有率を算出部で算出する工程とを主に備える。 [Viscosity measurement method]
The viscosity measuring method using the viscosity measuring device 1 includes the steps of heating the slurry in the slurry storage container 21 with the heating unit 3 and stirring with the stirrer 22, detecting the viscous resistance of the slurry, and evaporation from the slurry. The method mainly includes a step of collecting the solvent in a solvent recovery section 4 and measuring the amount of evaporation of the solvent, and a step of calculating the solvent content in the slurry from the amount of evaporation in a calculation section.

〔検出工程〕
粘性抵抗の検出工程では、スラリー貯留容器２１内のスラリーを加温部３で加温しつつ撹拌機２２で撹拌し、前記スラリーの粘性抵抗によるトルクを検出する。前記スラリーは、作業者がスラリー貯留容器２１内に予め投入してもよいし、当該粘度測定装置１がスラリー供給部５備え、このスラリー供給部５がスラリー貯留容器２１内に供給してもよい。前記スラリーは、加温部３で前記スラリーが含有する溶剤が蒸発する温度に加温される。スラリー貯留容器２１内の前記スラリーは、粘度測定の開始時に撹拌機２２の回転ロータの少なくとも一部が前記スラリーに浸漬される量が投入又は供給される。撹拌機２２はトルク検出器を有し、前記スラリーを撹拌するトルクを検出する。この検出されたトルクの値から前記スラリーの粘度を算出する。 [Detection process]
In the viscous resistance detection step, the slurry in the slurry storage container 21 is heated by the heating unit 3 and stirred by the stirrer 22, and the torque due to the viscous resistance of the slurry is detected. The slurry may be placed in advance into the slurry storage container 21 by an operator, or the viscosity measuring device 1 may include a slurry supply section 5, and the slurry supply section 5 may supply the slurry into the slurry storage container 21. . The slurry is heated in the heating section 3 to a temperature at which the solvent contained in the slurry evaporates. The slurry in the slurry storage container 21 is added or supplied in such an amount that at least a portion of the rotating rotor of the stirrer 22 is immersed in the slurry at the start of viscosity measurement. The stirrer 22 has a torque detector and detects the torque for stirring the slurry. The viscosity of the slurry is calculated from the detected torque value.

〔測定工程〕
蒸発溶剤の重量を測定する工程では、前記スラリーから蒸発する溶剤を溶剤回収部４で回収して前記溶剤の蒸発量を測定する。具体的には、スラリー貯留容器２１から排出される蒸発溶剤を、蒸発溶剤排出管Ｐ２を介して溶剤貯留容器４１に回収し、前記蒸発量を測定する。蒸発溶剤排出管Ｐ２の一部に凝縮機構４２が配設され、この凝縮機構４２によって液化された溶剤を測定するとよい。溶剤回収部４が、前記液化溶剤の重量を測定する重量測定機構４３を有し、溶剤貯留容器４１を重量測定機構４３に載置して前記液化溶剤の重量を経時的に測定するとよい。 [Measurement process]
In the step of measuring the weight of the evaporated solvent, the solvent evaporated from the slurry is collected by the solvent recovery section 4, and the amount of evaporated solvent is measured. Specifically, the evaporated solvent discharged from the slurry storage container 21 is collected into the solvent storage container 41 via the evaporated solvent discharge pipe P2, and the amount of evaporation is measured. It is preferable that a condensing mechanism 42 is disposed in a part of the evaporated solvent discharge pipe P2, and the solvent liquefied by this condensing mechanism 42 is measured. It is preferable that the solvent recovery unit 4 has a weight measuring mechanism 43 that measures the weight of the liquefied solvent, and that the solvent storage container 41 is placed on the weight measuring mechanism 43 to measure the weight of the liquefied solvent over time.

〔算出工程〕
算出工程では、前記溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出部で算出する。重量測定機構４３と撹拌機２２のトルク検出器とが前記算出部に測定値を送信可能に接続され、前記算出部が、入力された前記液化溶剤の重量と前記スラリーの粘性抵抗のトルク値とを記憶し、その経時的変化を表、グラフ等にして印刷、表示等できるとよい。 [Calculation process]
In the calculation step, the calculation unit calculates the solvent content in the slurry from the evaporation amount of the solvent. The weight measurement mechanism 43 and the torque detector of the stirrer 22 are connected to be able to send measured values to the calculation unit, and the calculation unit calculates the input weight of the liquefied solvent and the torque value of the viscous resistance of the slurry. It would be good if the changes over time could be stored and printed or displayed in a table, graph, etc.

［利点］
当該粘度測定装置１は、スラリーの粘度を測定する粘度測定部２と、粘度測定部２で測定される前記スラリーを加温する加温部３と、加温により蒸発する前記溶剤を回収する溶剤回収部４とを備えるため、前記スラリーの溶剤含有量及び粘度を同時に測定することができる。このため、前記スラリーの溶剤含有量と粘度との関係を容易に把握することができる。 [advantage]
The viscosity measuring device 1 includes a viscosity measuring section 2 that measures the viscosity of a slurry, a heating section 3 that heats the slurry measured by the viscosity measuring section 2, and a solvent that collects the solvent that evaporates due to heating. Since the slurry is equipped with a recovery section 4, the solvent content and viscosity of the slurry can be measured at the same time. Therefore, the relationship between the solvent content and viscosity of the slurry can be easily understood.

当該粘度測定装置１を用いてスラリーの溶剤含有量と粘度との関係を調査した。前記スラリーは、石炭と溶剤とを混合したペースト状混合物を加熱することにより石炭中の可溶成分を溶剤中に溶出させ、固液分離により可溶成分が溶け込んだ溶液を取り出したものであり、無灰炭と溶剤とを含む。前記溶剤の蒸発温度は２５０℃である。 The relationship between the solvent content and viscosity of the slurry was investigated using the viscosity measuring device 1. The slurry is obtained by heating a paste-like mixture of coal and a solvent to elute the soluble components in the coal into the solvent, and extracting a solution in which the soluble components have been dissolved by solid-liquid separation. Contains ashless charcoal and a solvent. The evaporation temperature of the solvent is 250°C.

スラリー貯留容器２１に前記スラリー投入し、加温して前記溶剤を蒸発させると共に、撹拌機２２で撹拌し、その回転トルクを検出した。前記スラリーは、２５０℃で加温し、前記スラリーの溶剤含有量が１ｗｔ％になったところで加温を停止した。加温を停止して暫くすると前記スラリーが固化したことが確認できた。試験開始時の前記スラリーは、粘度が約１０［ｍＰａ・ｓ］、溶剤含有率が約９０ｗｔ％であった。 The slurry was put into a slurry storage container 21, heated to evaporate the solvent, and stirred by a stirrer 22, and its rotational torque was detected. The slurry was heated at 250° C., and heating was stopped when the solvent content of the slurry reached 1 wt%. It was confirmed that the slurry had solidified a while after the heating was stopped. The slurry at the start of the test had a viscosity of about 10 [mPa·s] and a solvent content of about 90 wt%.

蒸発した溶剤は、凝縮機構４２で液化して溶剤貯留容器４１に回収し、この液化溶剤の重量を重量測定機構４３で測定して算出部で前記スラリーの溶剤含有率を算出した。溶剤の蒸発により前記スラリーの体積が減少した分はスラリー供給部５からスラリー貯留容器２１に継ぎ足し、常に撹拌機２２の回転ロータの全部が前記スラリーに浸っている状態を維持した。溶剤蒸発量から所定溶剤含有率に対し前記回転ロータを２００ｒｐｍ（せん断速度４５０ｓ－１）で回転させた際のトルクを測定して前記スラリーの粘度を算出した。 The evaporated solvent was liquefied by the condensation mechanism 42 and collected in the solvent storage container 41, the weight of this liquefied solvent was measured by the weight measuring mechanism 43, and the solvent content of the slurry was calculated by the calculation section. The volume of the slurry reduced due to evaporation of the solvent was added to the slurry storage container 21 from the slurry supply section 5, so that the entire rotor of the stirrer 22 was always immersed in the slurry. The viscosity of the slurry was calculated from the amount of solvent evaporation by measuring the torque when the rotor was rotated at 200 rpm (shear rate 450 s -1 ) for a predetermined solvent content.

試験の結果を図２，３に示す。この結果から、前記スラリーの溶剤含有量と粘度との関係は、下記式１の関係にあることが分かった。
η＝９．４×１０２・ｅｘｐ（－７．９・Ｓ） ・・・（１）
なお、ηは、粘度［ｍＰａ・ｓ］であり、Ｓは、前記スラリーの溶剤含有率［ｗｔ％］である。 The test results are shown in Figures 2 and 3. From this result, it was found that the relationship between the solvent content and viscosity of the slurry was expressed by the following formula 1.
η=9.4×10 2・exp(-7.9・S)...(1)
Note that η is the viscosity [mPa·s], and S is the solvent content rate [wt%] of the slurry.

［その他の実施形態］
前記実施形態は、本発明の構成を限定するものではない。従って、前記実施形態は、本明細書の記載及び技術常識に基づいて前記実施形態各部の構成要素の省略、置換又は追加が可能であり、それらは全て本発明の範囲に属するものと解釈されるべきである。 [Other embodiments]
The embodiments described above do not limit the configuration of the present invention. Therefore, in the embodiment, it is possible to omit, replace, or add components of each part of the embodiment based on the description in this specification and common general knowledge, and all of these are interpreted as falling within the scope of the present invention. Should.

粘度測定部２は、スラリー貯留容器２１内の圧力を変化できるように構成されてもよい。このようにすることで、例えば、通常では揮発してしまう溶剤を液体状態に保持しながら粘度測定をすることができる。 The viscosity measurement unit 2 may be configured to be able to change the pressure within the slurry storage container 21. By doing so, for example, the viscosity can be measured while keeping the solvent, which normally evaporates, in a liquid state.

本発明に係る粘度測定装置は、溶剤を含むスラリーの溶剤含有率と粘度との関係を容易に把握することができるため、スラリーを取り扱う現場やスラリーを取り扱う機器の開発において特に好適に利用することができる。 Since the viscosity measuring device according to the present invention can easily grasp the relationship between the solvent content and viscosity of a slurry containing a solvent, it is particularly suitable for use at sites where slurry is handled or in the development of equipment that handles slurry. I can do it.

１ 粘度測定装置
２ 粘度測定部
２１ スラリー貯留容器
２１ａ スラリー貯留容器本体
２１ｂ スラリー貯留容器蓋
２２ 撹拌機
３ 加温部
４ 溶剤回収部
４１ 溶剤貯留容器
４１ａ 溶剤貯留容器本体
４１ｂ 溶剤貯留容器蓋
４２ 凝縮機構
４３ 重量測定機構
５ スラリー供給部
Ｐ１ スラリー供給管
Ｐ２ 蒸発溶剤排出管
Ｐ３ 溶剤排出管 1 Viscosity measurement device 2 Viscosity measurement section 21 Slurry storage container 21a Slurry storage container main body 21b Slurry storage container lid 22 Stirrer 3 Heating section 4 Solvent recovery section 41 Solvent storage container 41a Solvent storage container main body 41b Solvent storage container lid 42 Condensation mechanism 43 Weight measurement mechanism 5 Slurry supply section P1 Slurry supply pipe P2 Evaporated solvent discharge pipe P3 Solvent discharge pipe

Claims (4)

溶剤を含むスラリーの粘度測定装置であって、
前記スラリーの粘度を測定する粘度測定部と、
前記粘度測定部で測定される前記スラリーを加温する加温部と、
前記加温により蒸発した前記溶剤を回収する溶剤回収部と、
前記溶剤の蒸発量から前記スラリーにおける溶剤含有率を算出する算出部と
を備える粘度測定装置。 A device for measuring the viscosity of a slurry containing a solvent,
a viscosity measurement unit that measures the viscosity of the slurry;
a heating section that heats the slurry measured by the viscosity measuring section;
a solvent recovery unit that recovers the solvent evaporated by the heating;
A calculation unit that calculates the solvent content in the slurry from the evaporation amount of the solvent. 前記溶剤回収部が、前記蒸発した溶剤を液化する凝縮機構を有する請求項１に記載の粘度測定装置。 The viscosity measuring device according to claim 1, wherein the solvent recovery section includes a condensation mechanism that liquefies the evaporated solvent. 前記溶剤回収部が、前記凝縮機構で液化された溶剤の重量を測定する重量測定機構をさらに有する請求項２に記載の粘度測定装置。 The viscosity measuring device according to claim 2, wherein the solvent recovery section further includes a weight measuring mechanism that measures the weight of the solvent liquefied by the condensing mechanism . 前記溶剤含有率が所定の閾値以下でスラリーを前記粘度測定部に追加するスラリー供給部をさらに備える請求項１、請求項２又は請求項３に記載の粘度測定装置。
 The viscosity measurement device according to claim 1, further comprising a slurry supply section that adds slurry to the viscosity measurement section when the solvent content is equal to or less than a predetermined threshold value.
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JP2007091526A (en) 2005-09-28 2007-04-12 Nippon Shokubai Co Ltd Method of manufacturing ceramic green sheet
JP2015132011A (en) 2013-12-11 2015-07-23 新日鐵住金株式会社 Oil content separating method, and oil content separating device
JP2017095619A (en) 2015-11-25 2017-06-01 株式会社神戸製鋼所 Method for producing ashless coals

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* Cited by examiner, † Cited by third party
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JPH0224103A (en) * 1988-07-12 1990-01-26 Mitsubishi Electric Corp Adjuster of viscosity
JPH11262724A (en) * 1998-03-18 1999-09-28 Miura Co Ltd Method and apparatus for regeneration of resist composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002274952A (en) 2001-03-16 2002-09-25 Hitachi Metals Ltd Vacuum deaerator and slurry deaeration process
JP2007091526A (en) 2005-09-28 2007-04-12 Nippon Shokubai Co Ltd Method of manufacturing ceramic green sheet
JP2015132011A (en) 2013-12-11 2015-07-23 新日鐵住金株式会社 Oil content separating method, and oil content separating device
JP2017095619A (en) 2015-11-25 2017-06-01 株式会社神戸製鋼所 Method for producing ashless coals

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