JPH0215014B2 - - Google Patents
Info
- Publication number
- JPH0215014B2 JPH0215014B2 JP8284282A JP8284282A JPH0215014B2 JP H0215014 B2 JPH0215014 B2 JP H0215014B2 JP 8284282 A JP8284282 A JP 8284282A JP 8284282 A JP8284282 A JP 8284282A JP H0215014 B2 JPH0215014 B2 JP H0215014B2
- Authority
- JP
- Japan
- Prior art keywords
- reaction
- water tank
- tube
- temperature
- tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 98
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 239000012495 reaction gas Substances 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 5
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 description 8
- 239000003245 coal Substances 0.000 description 5
- 238000004891 communication Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Description
【発明の詳細な説明】
本発明は、固体と気体との反応熱、例えば、石
炭と水素との反応熱を測定するための装置に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for measuring the heat of reaction between a solid and a gas, such as the heat of reaction between coal and hydrogen.
従来、物質の燃焼熱を測定するための熱量計は
種種市販され、かつ、その測定精度も比較的高い
が、固体と気体との反応熱を精度よく測定する反
応熱測定装置は、装置化の困難なガスの流通系を
必要とすることもあつて、未だ開発されていな
い。しかしながら、固体と気体の反応熱を精度よ
く測定することは、両者の反応の機構を解明する
上で非常に重要な意味を有し、その開発が強く要
望されている。 Conventionally, various types of calorimeters for measuring the heat of combustion of substances are commercially available, and their measurement accuracy is relatively high. It has not yet been developed because it requires a difficult gas distribution system. However, accurate measurement of the heat of reaction between a solid and a gas has a very important meaning in elucidating the reaction mechanism between the two, and its development is strongly desired.
本発明者は、固体と気体との反応熱測定装置を
開発すべく鉛意研究を重ねた結果、本発明を完成
するに到つた。 The present inventor has completed the present invention as a result of repeated research aimed at developing an apparatus for measuring reaction heat between a solid and a gas.
すなわち、本発明によれば、円筒状の試料セル
内に、上端を貫いて反応温度測定用の熱電対を立
設し、周面上部に反応ガス流通孔を設けた固体試
料を封入させる円筒状の反応管を、その外側にヒ
ータを備えた加熱管、筒状の反射板、反応ガスの
熱交換用らせん管を順次同心的に設け、かつ上記
らせん管の先端を加熱管の下方内部に開口させて
封入するとともに、この試料セルを円筒状の水槽
内に取付保持し、かつこの水槽内には、試料セル
下端から水槽内周面に沿つて水槽上部に開く生成
ガスの熱交換用らせん管、撹拌棒、水温測定用の
熱電対を各設け、さらに上記水槽を反応ガス熱交
換用のらせん管、攪拌機構、加熱機構及び温度検
知用熱電対を有する外部水槽内に設けるととも
に、外部には、前記内槽に設けた熱電対、前記外
槽に設けた熱電対及び前記外槽に設けた加熱機構
に各接続する自動温度調節器及び前記試料セル内
に設けたヒータに接続する電流計を設けたことを
特徴とする反応熱測定装置が提供される。 That is, according to the present invention, a cylindrical sample cell is provided with a thermocouple for measuring reaction temperature erected through the upper end thereof, and a solid sample is enclosed in the cylindrical sample cell with reaction gas flow holes provided in the upper part of the circumference. A heating tube equipped with a heater, a cylindrical reflection plate, and a spiral tube for heat exchange of reaction gas are sequentially and concentrically arranged on the outside of the reaction tube, and the tip of the spiral tube is opened inside the heating tube below. At the same time, this sample cell is installed and held in a cylindrical water tank, and inside this water tank, there is a spiral tube for heat exchange of the generated gas that opens from the bottom end of the sample cell to the top of the tank along the inner peripheral surface of the tank. , a stirring rod, and a thermocouple for measuring water temperature, and the above-mentioned water tank is installed in an external water tank that has a spiral tube for reaction gas heat exchange, a stirring mechanism, a heating mechanism, and a thermocouple for temperature detection. , an automatic temperature controller connected to the thermocouple provided in the inner tank, a thermocouple provided in the outer tank, and a heating mechanism provided in the outer tank, and an ammeter connected to a heater provided in the sample cell. A reaction heat measuring device is provided.
本発明の実施例を図面について説明すると、第
１図は外部水槽を除いた要部を示し、１は試料セ
ルであつて、外周面にフイン２が列設され、下端
は同じくフインを有する小径のフイルター収容部
３に形成されている。この試料セル１は、水槽４
内に適宜の取付具（図示せず）を介して吊設保持
されており、水槽４の蓋部を貫いて設けた反応ガ
ス導入管５を介して後述する外部水槽１９内の反
応ガス熱交換用らせん管２３で一定温度に調節さ
れた反応ガスが送り込まれ、またフイルター収容
部３底部から生成ガスが水槽４の内周面に沿うら
せん管６を通つて水槽４上部の生成ガス排出管７
により取り出されるようになつている。 To explain an embodiment of the present invention with reference to the drawings, Fig. 1 shows the main parts excluding the external water tank, 1 is a sample cell, and fins 2 are arranged in a row on the outer circumferential surface, and the lower end has a small diameter that also has fins. It is formed in the filter accommodating part 3 of. This sample cell 1 has a water tank 4
The reactant gas heat exchanger inside the external water tank 19 (described later) is carried out via a reactant gas inlet pipe 5 provided through the lid of the water tank 4. A reactant gas whose temperature is adjusted to a constant temperature is fed into the helical tube 23, and the produced gas flows from the bottom of the filter accommodating section 3 through a helical tube 6 along the inner circumferential surface of the water tank 4 to a produced gas discharge pipe 7 at the top of the water tank 4.
It is now being taken out by
試料セル１の内部には、その蓋部に上部を接続
し、下端をフイルター収容部３に接続した１つの
立管よりなる反応管８が画設され、内部に設けた
目皿９上に固形試料（例えば石炭）を封入するよ
うになつている。この反応管８の外側には外周面
にヒータ１０を巻装した加熱管１１が上下端を密
封して重合され、さらにその外側を間隔をおいて
ステンレス板よりなる円筒状の反射板１２が取り
囲んでいる。前記反応ガス導入管５は、この反射
板１２を取りまくらせん管１３を経て加熱管１１
の下方の内部に開口しており、反応ガスは、加熱
管１１と反応管８の間を通つて上昇し、反応管８
の上部周面に横列した反応ガス流通孔１４を通つ
て反応管８内に流入するようになつている。水槽
４の上面には、蓋部を貫いて前記反応ガス導入管
５、生成ガス排出管７、ヒータ１０に連なる電極
１５のほかに、下端を試料セル１内の試料内に位
置した反応温度測定用の熱電対１６、水槽４の水
温測定用の熱電対１７ならびに水槽４内に垂下取
付され上端を適宜の動力に接続して回転される撹
拌棒１８が各々突設されており、それらの取付部
は水槽４と密封状態に作られている。 Inside the sample cell 1, a reaction tube 8 consisting of a standpipe whose upper end is connected to its lid and whose lower end is connected to the filter accommodating section 3 is defined. It is designed to enclose a sample (for example, coal). On the outside of this reaction tube 8, a heating tube 11 having a heater 10 wrapped around its outer circumferential surface is superimposed with its upper and lower ends sealed, and a cylindrical reflecting plate 12 made of a stainless steel plate is surrounded at intervals on the outside. I'm here. The reaction gas introduction pipe 5 passes through a spiral pipe 13 surrounding this reflection plate 12 and then connects to a heating pipe 11.
The reactant gas passes through between the heating tube 11 and the reaction tube 8 and rises into the reaction tube 8.
The reaction gas flows into the reaction tube 8 through reaction gas flow holes 14 arranged horizontally on the upper circumferential surface of the reaction tube 8 . On the upper surface of the water tank 4, in addition to an electrode 15 that penetrates through the lid and connects to the reaction gas introduction pipe 5, generated gas discharge pipe 7, and heater 10, there is also an electrode 15 located at the lower end within the sample in the sample cell 1 for measuring the reaction temperature. A thermocouple 16 for measuring water temperature in the water tank 4, a thermocouple 17 for measuring the water temperature in the water tank 4, and a stirring rod 18 that is installed hanging down inside the water tank 4 and rotated by connecting the upper end to an appropriate power source are protruded from each other. The part is made in a sealed state with the water tank 4.
上記第１図に示す部分は、前記したように、さ
らに外部水槽に収容して一体に組立てられる。す
なわち、第２図において、１９は外部水槽であつ
て加熱機構２０、温度検知機構２１、撹拌機構２
２、反応ガス熱交換用らせん管２３を備え、さら
に液面リレー２４を介して前記水槽４内に所要の
水位まで外部水槽内の水を供給するための外部水
槽１９と連通する電磁弁２５付き連通管２６を有
している。反応ガス熱交換用らせん管２３は、外
部より供給される反応ガス（例えば水素）を外部
水槽１９内の水と同じ温度まで熱交換したのち、
前記反応ガス導入管５に接続する。なお、２７は
自動温度調節器、２８は温度記録計であり、２９
は水量設定用の電気接点である。３０は断熱容器
であり、断熱材３１を内面に張装して水槽４から
外部へ熱の流出を遮断する。３２は反応温度調節
器、３３は電流計である。 As described above, the parts shown in FIG. 1 are further housed in an external water tank and assembled together. That is, in FIG. 2, 19 is an external water tank, which includes a heating mechanism 20, a temperature detection mechanism 21, and a stirring mechanism 2.
2. Equipped with a helical pipe 23 for reaction gas heat exchange, and further equipped with an electromagnetic valve 25 communicating with the external water tank 19 for supplying water in the external water tank to the required water level in the water tank 4 via a liquid level relay 24. It has a communication pipe 26. The reaction gas heat exchange spiral tube 23 heat-exchanges the reaction gas (for example, hydrogen) supplied from the outside to the same temperature as the water in the external water tank 19, and then
Connected to the reaction gas introduction pipe 5. In addition, 27 is an automatic temperature controller, 28 is a temperature recorder, and 29
is an electrical contact for setting the water amount. 30 is a heat insulating container, and the inner surface is covered with a heat insulating material 31 to block heat from flowing out from the water tank 4 to the outside. 32 is a reaction temperature regulator, and 33 is an ammeter.
本発明は上記のように構成され、試料セル１内
に目皿９上に一定量の粉末状の固体、例えば石炭
を封入し、試料セル１を水槽４内に設入させると
ともに、その全体を断熱容器３０に収容して第２
図のように外部水槽１９内に収容する。 The present invention is constructed as described above, in which a certain amount of powdered solid, such as coal, is sealed on the perforated plate 9 in the sample cell 1, and the sample cell 1 is placed in the water tank 4, and the entire sample cell 1 is placed in the water tank 4. The second
It is housed in an external water tank 19 as shown in the figure.
次に、外部水槽１９内に水を温度検知機構２１
と自動温度調節器２７の作用により、所要の温
度、例えば20℃に保持した後、電磁弁２５を開
き、落差などを利用して外部水槽水の一部を連通
管２６により水槽４内に導入する。その際、連通
管２６は外部水槽水中を通過しているため水の調
整温度には変動がない。水槽４内の水量設定の電
気接点２９を所定位置に設定しておくことによ
り、水槽４の水位はこの点まで上昇し、水位がこ
の電気接点の位置に達すると、液面リレー２４が
作動して電磁弁２５は閉になる。従つて、この操
作により、外部水槽内の一定温度に調整された水
を常に一定量水槽４内に自動的に秤量することが
できる。 Next, water is poured into the external water tank 19 by the temperature detection mechanism 21.
After maintaining the required temperature, for example, 20 degrees Celsius, by the action of the automatic temperature controller 27, the solenoid valve 25 is opened, and a portion of the external tank water is introduced into the tank 4 through the communication pipe 26 using a drop or the like. do. At this time, since the communication pipe 26 passes through the water in the external aquarium, there is no change in the adjusted temperature of the water. By setting the electrical contact 29 for setting the water volume in the water tank 4 to a predetermined position, the water level in the water tank 4 will rise to this point, and when the water level reaches the position of this electrical contact, the liquid level relay 24 will be activated. Then, the solenoid valve 25 is closed. Therefore, by this operation, a constant amount of water adjusted to a constant temperature in the external water tank can be automatically weighed into the water tank 4 at all times.
前記のようにして測定準備が終つた後、電極１
５から電気を通じてヒータ１０を発熱させ、加熱
管１１及び反応管８を介して反応管８内の固体試
料を加熱する。この場合、ヒータに通電した電気
量は電流計３３により記録される。固体試料の温
度は熱電対１６により測定され、温度記録計によ
り記録される。 After completing the measurement preparation as described above, the electrode 1
The heater 10 generates heat through electricity from 5, and the solid sample in the reaction tube 8 is heated through the heating tube 11 and the reaction tube 8. In this case, the amount of electricity supplied to the heater is recorded by the ammeter 33. The temperature of the solid sample is measured by a thermocouple 16 and recorded by a temperature recorder.
試料温度が所定の反応温度に達した時に、反応
ガスを外部水槽１９内の熱交換用らせん管２３を
通じて反応ガス導入管５から導入する。この反応
ガスはらせん管１３を通り、下部らせん管の出口
を通つて反応管８と加熱管１１との間の空隙部に
入り、この空隙部を上昇し、その間に所要の反応
温度に加熱される。そして、この加熱された反応
ガスは、反応管の上部周囲に横列した反応ガス流
通孔１４から反応管８内部に入り、固体試料と接
触反応する。 When the sample temperature reaches a predetermined reaction temperature, a reaction gas is introduced from the reaction gas introduction pipe 5 through the heat exchange spiral pipe 23 in the external water tank 19. This reaction gas passes through the helical tube 13, enters the gap between the reaction tube 8 and the heating tube 11 through the outlet of the lower helical tube, rises through this gap, and is heated to the required reaction temperature in the meantime. Ru. The heated reaction gas then enters the inside of the reaction tube 8 through the reaction gas flow holes 14 arranged horizontally around the upper part of the reaction tube, and comes into contact with the solid sample to react.
前記の接触反応により得られる生成ガスは、反
応管下部からフイルター収容部３を通り、その内
部のフイルター（例えば石英綿、脱脂綿などの充
填層）と接触し、生成ガス中に含まれる液状成分
がここで除去される。液状成分の除去された生成
ガスは、らせん管６を通つて水槽４の温度まで冷
却された後、生成ガス排出管７から排出される。
前記装置において、反応温度（試料の温度）は、
熱電対１６とヒータ電極１５に接続する反応温度
調節器３２により所定の温度に調節され、その温
度は、時間に対して記録される。また、水槽４の
温度が反応経過と共に上昇すると、自動温度調節
器２７と、それに接続する水槽４の水温測定用の
熱電対１７及び外部水槽水に対する温度検知機構
２１の熱電対と加熱機構２０との協働作用によ
り、外部水槽１９の水温は水槽４の水温に追随し
て上昇する。この温度制御によつて、外部水槽１
９の水温は常に水槽４の水温とほぼ等しい温度に
保持され、水槽４からの熱の逃散が防止され、ま
た反応ガスも熱交換用らせん管２３により水槽１
９内の水温にほぼ等しくなつてから水槽４内に供
給されるので、水槽４の効果的な断熱が達成され
る。 The product gas obtained by the above-mentioned contact reaction passes through the filter housing part 3 from the lower part of the reaction tube, contacts the filter (for example, a packed layer of quartz wool, absorbent cotton, etc.) inside the filter, and the liquid components contained in the product gas are removed. removed here. The generated gas from which the liquid components have been removed passes through the spiral pipe 6 and is cooled to the temperature of the water tank 4, and then is discharged from the generated gas exhaust pipe 7.
In the device, the reaction temperature (temperature of the sample) is
A predetermined temperature is regulated by a reaction temperature regulator 32 connected to the thermocouple 16 and the heater electrode 15, and the temperature is recorded over time. Further, when the temperature of the water tank 4 rises as the reaction progresses, the automatic temperature controller 27, the thermocouple 17 for measuring the water temperature of the water tank 4 connected thereto, the thermocouple of the temperature detection mechanism 21 for external water tank water, and the heating mechanism 20 Due to the cooperative action of the above, the water temperature in the external water tank 19 increases following the water temperature in the water tank 4. By this temperature control, the external water tank 1
The water temperature in water tank 9 is always maintained at approximately the same temperature as the water temperature in water tank 4, preventing heat from escaping from water tank 4, and the reaction gas is also transferred to water tank 1 through heat exchange spiral pipe 23.
Since the water is supplied into the water tank 4 after the water temperature becomes approximately equal to that in the water tank 9, effective insulation of the water tank 4 is achieved.
前記のようにして反応を所定時間行つた後、反
応を停止させる。即ち、反応ガスの導入、生成ガ
スの導出及びヒータ１０の加熱をそれぞれ停止さ
せる。次いで、水槽４の水温の上昇が見られなく
なつた時の、その水温を測定し、測定を終了す
る。 After the reaction has been carried out for a predetermined period of time as described above, the reaction is stopped. That is, the introduction of the reaction gas, the discharge of the generated gas, and the heating of the heater 10 are stopped. Next, the water temperature in the water tank 4 is measured when no increase in water temperature is observed, and the measurement is completed.
前記のようにして測定を行つた場合、水槽４内
の水に加えられた全熱量Ｑは次の式で表わされ
る。 When the measurement is performed as described above, the total amount of heat Q added to the water in the water tank 4 is expressed by the following equation.
全熱量Qcal＝（W1＋W2）×△Ｔ （）
W1……水槽４の水量（ｇ）
W2……装置水当量（ｇ）
△Ｔ……測定前後の水槽４内の水温の差
また、水槽４内に導入された全熱量Ｑ（cal）
は、固体試料と反応ガスとの反応による反応熱
と、ヒータ１０により導入されたジユール熱と、
反応ガスと生成ガスとの顕熱との差に相当する熱
とを基準にすると、次の式で表わすことができ
る。Total heat Qcal = (W 1 + W 2 ) × △T () W 1 ...Amount of water in tank 4 (g) W 2 ... Equipment water equivalent (g) △T ... Difference in water temperature in tank 4 before and after measurement Also, the total amount of heat Q (cal) introduced into the water tank 4
is the reaction heat due to the reaction between the solid sample and the reaction gas, the Joule heat introduced by the heater 10,
Based on the heat corresponding to the difference in sensible heat between the reaction gas and the produced gas, it can be expressed by the following equation.
Ｑ（cal）＝q1＋q2＋q3 （）
q1……反応熱
q2……ジユール熱
q3……反応ガスと生成ガスの顕熱の差
従つて、前記（）及び（）の式から、反応
熱q1は次の式で表わされる。 Q (cal) = q 1 + q 2 + q 3 () q 1 ...Heat of reaction q 2 ...Jeur's heat q 3 ...Difference between the sensible heats of the reaction gas and the produced gas Therefore, the above equations () and () Therefore, the heat of reaction q 1 is expressed by the following formula.
q1＝Ｑ−（q2＋q3）
＝（W1＋W2）×△Ｔ−（q2＋q3）
即ち、反応熱q1は、水槽４の水の量W1、装置
水当量W2、水槽４の水の温度上昇△Ｔ、ジユー
ル熱q2及び反応ガスと生成ガスの顕熱の差q3をそ
れぞれ測定することによつて求めることができ
る。この場合、水槽４内の水の量W1、及び装置
水当量W2は装置因子としてあらかじめ決定され
るので定数として扱われ、また反応ガスと生成ガ
スの顕熱の差q3は、それぞれのガスはいずれも水
槽４内の水温とほぼ等しい温度で導入及び導出さ
れるので、実質上無視することが可能である。従
つて、本発明の装置によれば、反応熱q1は、水槽
４内の水温上昇△Ｔと、ジユール熱q2とを測定す
ることによつて得ることができる。なお、ジユー
ル熱q2は、前記電流計３３の記録に基づき、次式
に求められる。q 1 = Q - (q 2 + q 3 ) = (W 1 + W 2 ) x △T - (q 2 + q 3 ) In other words, the heat of reaction q 1 is the amount of water in the water tank 4 W 1 , the water equivalent of the device W 2 , the temperature rise ΔT of the water in the water tank 4, the Joule heat q 2 and the difference q 3 between the sensible heats of the reaction gas and the produced gas. In this case, the amount of water W 1 in the water tank 4 and the equipment water equivalent W 2 are determined in advance as equipment factors, so they are treated as constants, and the difference q 3 in sensible heat between the reaction gas and the produced gas is Since both gases are introduced and led out at approximately the same temperature as the water temperature in the water tank 4, they can be substantially ignored. Therefore, according to the apparatus of the present invention, the reaction heat q 1 can be obtained by measuring the water temperature rise ΔT in the water tank 4 and the Joule heat q 2 . Note that the Joule heat q 2 is determined by the following formula based on the record of the ammeter 33.
q2＝∫t 0I2Rdt （）
Ｉ……アンペア
Ｒ……ヒータの抵抗（Ω）
ｔ……通電時間（秒）
本発明は以上説明したように、一定量の水の温
度上昇の測定と、外部に設けた電流計によるジユ
ール熱の測定とにより反応熱を知るものであり、
特に圧入すべき反応ガスを、反射板１２を取りま
くらせん管１３を介して加熱管１１の下方内部に
供給し、反応管８外周に沿つて上昇させたのち反
応ガス流通孔１４から反応管８内に入るようにし
たから、反応熱測定に際しての加熱時における試
料セル１内の気体の熱膨張を反応ガス流通孔１４
を介して生成ガス側に逃がし、試料セルの内圧の
上昇を防ぐことができるとともに、上記らせん管
１３はヒータ１０の反応ガスへの伝熱を助長し、
かつフイン２と共働して加熱終了後の試料セル１
の冷却を促し、測定誤差が生じないようにする利
点がある。 q 2 =∫ t 0 I 2 Rdt () I...Ampere R...Heater resistance (Ω) t...Electrification time (seconds) As explained above, the present invention measures the temperature rise of a certain amount of water. The reaction heat can be determined by measuring the Joule heat using an external ammeter.
In particular, the reaction gas to be pressurized is supplied to the lower interior of the heating tube 11 through the spiral tube 13 surrounding the reflection plate 12, and after rising along the outer circumference of the reaction tube 8, the reaction gas is introduced into the reaction tube 8 from the reaction gas distribution hole 14. The thermal expansion of the gas in the sample cell 1 during heating during reaction heat measurement is measured by the reaction gas flow hole 14.
The helical tube 13 facilitates heat transfer from the heater 10 to the reaction gas, and prevents an increase in the internal pressure of the sample cell.
In addition, the sample cell 1 after heating is cooperated with the fin 2.
This has the advantage of promoting cooling and preventing measurement errors.
本発明は、種々の固体と気体との反応系、例え
ば石炭の水素化反応、石炭の乾留、バイオマス、
産業用廃棄物の熱分解、種々の金属鉱石のバイ焼
などにおける反応熱の測定に対して有利に適用さ
れる。 The present invention is applicable to reaction systems between various solids and gases, such as coal hydrogenation reaction, coal carbonization, biomass,
It is advantageously applied to measuring the heat of reaction in the thermal decomposition of industrial waste, the bi-burning of various metal ores, etc.
第１図は、本発明の要部を示す縦断面図、第２
図は全体説明図である。
図中符号、１は試料セル、２はフイン、３はフ
イルター収容部、４は内部水槽、５は反応ガス導
入管、６はらせん管、７は生成ガス排出管、８は
反応管、９は目皿、１０はヒータ、１１は加熱
管、１２は反射板、１３はらせん管、１４は反応
ガス流通孔、１６は熱電対、１７は温度計、１８
は撹拌棒、１９は外部水槽、２３は反応ガス熱交
換用らせん管、２６は連通管、２７は自動温度調
節器、２９は電気接点、３０は断熱容器、３２は
反応温度調節器、３３は電流計である。
FIG. 1 is a vertical cross-sectional view showing the main parts of the present invention, and FIG.
The figure is an overall explanatory diagram. Codes in the figure: 1 is a sample cell, 2 is a fin, 3 is a filter housing part, 4 is an internal water tank, 5 is a reaction gas introduction pipe, 6 is a spiral pipe, 7 is a produced gas discharge pipe, 8 is a reaction tube, 9 is a Perforated plate, 10 is a heater, 11 is a heating tube, 12 is a reflection plate, 13 is a spiral tube, 14 is a reaction gas flow hole, 16 is a thermocouple, 17 is a thermometer, 18
19 is a stirring rod, 19 is an external water tank, 23 is a spiral tube for reaction gas heat exchange, 26 is a communication tube, 27 is an automatic temperature controller, 29 is an electric contact, 30 is a heat insulating container, 32 is a reaction temperature controller, 33 is a It is an ammeter.
Claims (1)
度測定用の熱電対を立設し、周面上部に反応ガス
流通孔を設けた固体試料を封入させる円筒状の反
応管を、その外側にヒータを備えた加熱管、筒状
の反射板、反応ガスの熱交換用らせん管を順次同
心的に設け、かつ上記らせん管の先端を加熱管の
下方内部に開口させて封入するとともに、この試
料セルを円筒状の水槽内に取付保持し、かつこの
水槽内には、試料セル下端から水槽内周面に沿つ
て水槽上部に開く生成ガスの熱交換用らせん管、
攪拌棒、水温測定用の熱電対を各設け、さらに、
上記水槽を外部水槽内に設けるとともに、この外
部水槽には、前記反応管に接続する反応ガス熱交
換用らせん管、攪拌機構、加熱機構及び温度検知
用熱電対を各設け、さらに外部には、前記内槽に
設けた熱電対、前記外槽に設けた熱電対及び前記
外槽に設けた加熱機構に各接続する自動温度調節
器及び前記試料セル内に設けたヒータに接続する
電流計を各設けたことを特徴とする反応熱測定装
置。1 Inside a cylindrical sample cell, a thermocouple for measuring the reaction temperature is erected through the upper end, and a cylindrical reaction tube to enclose a solid sample with reaction gas flow holes provided at the upper part of the circumference is placed outside the cylindrical sample cell. A heating tube equipped with a heater, a cylindrical reflection plate, and a spiral tube for heat exchange of reaction gas are sequentially and concentrically installed in the tube, and the tip of the spiral tube is opened and sealed inside the heating tube. The sample cell is installed and held in a cylindrical water tank, and in this water tank there is a spiral pipe for heat exchange of the produced gas that opens from the bottom end of the sample cell to the top of the tank along the inner peripheral surface of the tank.
A stirring rod and a thermocouple for measuring water temperature are installed, and
The above-mentioned water tank is provided in an external water tank, and this external water tank is provided with a spiral tube for reaction gas heat exchange connected to the reaction tube, a stirring mechanism, a heating mechanism, and a thermocouple for temperature detection. A thermocouple provided in the inner tank, a thermocouple provided in the outer tank, an automatic temperature controller connected to the heating mechanism provided in the outer tank, and an ammeter connected to the heater provided in the sample cell, respectively. A reaction heat measuring device characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8284282A JPS58200147A (en) | 1982-05-17 | 1982-05-17 | Reaction heat measuring apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8284282A JPS58200147A (en) | 1982-05-17 | 1982-05-17 | Reaction heat measuring apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58200147A JPS58200147A (en) | 1983-11-21 |
| JPH0215014B2 true JPH0215014B2 (en) | 1990-04-10 |
Family
ID=13785641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8284282A Granted JPS58200147A (en) | 1982-05-17 | 1982-05-17 | Reaction heat measuring apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58200147A (en) |
-
1982
- 1982-05-17 JP JP8284282A patent/JPS58200147A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58200147A (en) | 1983-11-21 |
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