JPS62223669A - Method and device for automatic test of catalyst - Google Patents
Method and device for automatic test of catalystInfo
- Publication number
- JPS62223669A JPS62223669A JP6779086A JP6779086A JPS62223669A JP S62223669 A JPS62223669 A JP S62223669A JP 6779086 A JP6779086 A JP 6779086A JP 6779086 A JP6779086 A JP 6779086A JP S62223669 A JPS62223669 A JP S62223669A
- Authority
- JP
- Japan
- Prior art keywords
- trap
- liquid nitrogen
- collected
- reaction product
- valve
- 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.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 10
- 238000012360 testing method Methods 0.000 title claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 4
- 239000011344 liquid material Substances 0.000 claims abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 229910001872 inorganic gas Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
イ）産業上の利用分野
本発明は触媒自動試験方法及び装置に関するもので、工
業用触媒の反応性、耐久性等の性能、試験、評価を自動
的に行なうためのものである。[Detailed description of the invention] A) Industrial application field The present invention relates to an automatic catalyst testing method and device, which is used to automatically test and evaluate the performance, such as reactivity and durability, of industrial catalysts. It is something.
口）従来の技術
触媒試験装置としては、流通性反応装置、パルス反応部
を用いた装置が用いられているが、単独に使用されるた
め広範囲の成分分析例えばＨ２、Ｃ１−Ｃ１５の成分分
析をするのに一回のサンプリングでは足りず、回数が多
く必要である。(1) Conventional technology catalyst testing equipment uses a flow reactor or a device using a pulse reaction section, but since they are used alone, it is difficult to perform a wide range of component analysis, such as H2, C1-C15 component analysis. For this purpose, one sampling is not enough; many samplings are required.
ハ）解決すべき問題点
このため試料量を多く必要とし、その分析に手間と時間
がかかると共にガス体試料、液体試料を任意に測定する
ことも又連続的自動分析も行なうことが出来ず、更に高
分離能分析もなし得なかった。c) Problems to be solved For this reason, a large amount of sample is required, and the analysis thereof is laborious and time-consuming, and it is not possible to arbitrarily measure gas samples and liquid samples, and it is not possible to perform continuous automatic analysis. Furthermore, high-resolution analysis was not possible.
二）問題点を解決するための手段
バツクドカラム（Ｈ２，Ｃ１〜ｃ３の測定用）と、液相
化学結合型フユーズドシリ力キャビラリー力ラム（Ｃ４
〜Ｃ１５の測定用）の組合せが出来、コールドトラップ
の採用にょり一回のサンプリングでＨ２，Ｃ１〜Ｃ１５
の成分を一回で分析出来るようにし、且測定成分の分析
はＨ２，Ｃ１〜Ｃ１５に限定されず、カラム交換により
他成分の分析も可能にしたもので、気体又は液体材料を
触媒反応装置により触媒反応させた反応生成部分を液体
窒素を用いたトラップに導入し、水素部分はスルーさせ
て他の部分は捕集した後加熱脱着し、夫々ガスクロマト
グラフ部に導くことを特徴とする。2) Means to solve the problem Backed column (for measurement of H2, C1 to C3) and liquid phase chemically bonded fused silicon capillary column (C4
By using a cold trap, H2, C1 to C15 can be measured in one sampling.
In addition, the analysis of the components to be measured is not limited to H2, C1 to C15, and it is also possible to analyze other components by replacing the column. It is characterized in that the reaction product part subjected to the catalytic reaction is introduced into a trap using liquid nitrogen, the hydrogen part is allowed to pass through, and the other part is collected, heated and desorbed, and then guided to the gas chromatograph section.
ホ）実施例
１は、触媒再生時に用いる空気と実際の反応分析に用い
るＨｅとを切り換へる切換弁であり、２は、前記波体の
流量を制御するサーマルマスフローコントローラーであ
る。このサーマルマスフローコントローラー２は、外部
からの流量設定が可能であること当然である。３は、気
体試料を注入部６に送出する切換弁である。該切換弁は
ボート１６を接続し、該ボート１６から気体試料を流し
て検量管４に満たし切換弁３を切り換へることによって
注入部６に気体材料を送るようにしである５は、オート
サンプラーで、一定量の液体試料を注入部６に自動的に
送出する如く構成しである。注入部６は液体試料を気化
させる機能を持つ。e) Example 1 is a switching valve that switches between air used during catalyst regeneration and He used for actual reaction analysis, and 2 is a thermal mass flow controller that controls the flow rate of the wave body. It goes without saying that this thermal mass flow controller 2 can set the flow rate from the outside. 3 is a switching valve that sends the gas sample to the injection section 6. The switching valve is connected to a boat 16, and the gas sample is flowed from the boat 16 to fill the calibration tube 4, and the switching valve 3 is switched to send the gaseous material to the injection part 6. The sampler is configured to automatically deliver a fixed amount of liquid sample to the injection section 6. The injection part 6 has a function of vaporizing the liquid sample.
７は１反応炉であり、触媒は石英製の反、応管に積めら
れてここに挿入されている。この反応炉７は、外部から
設定温度を変更する事ができるのがよく、パルス反応炉
を用いることがよい。7 is a reactor, and the catalyst is loaded in a reaction tube made of quartz and inserted therein. It is preferable that the set temperature of the reactor 7 can be changed from the outside, and a pulse reactor is preferably used.
８は、切換弁で、実際の反応成分をトラップ部４に送出
する場合と、触媒の再生時に反応炉から流れてくる処理
ガスを系外に送出する場合とを切り換へる作用を有する
。また後者の場合、ガスクロマトグラフ部１２．１３の
検量線を作成する時に、切換弁１４によって標準ガスを
トラップ部１１に導入することができる。この場合、標
準ガスをボート１７から流して検量管１５に満たして切
換弁１４を切り換へることによってなされる。Reference numeral 8 denotes a switching valve which has the function of switching between sending the actual reaction components to the trap section 4 and sending out the processing gas flowing from the reactor during catalyst regeneration to the outside of the system. In the latter case, standard gas can be introduced into the trap section 11 by the switching valve 14 when creating a calibration curve for the gas chromatograph section 12.13. In this case, standard gas is flowed from the boat 17 to fill the calibration tube 15 and the switching valve 14 is switched.
９は、トラップ部１１を流通系、密閉系に切り換へる切
換弁である。Reference numeral 9 denotes a switching valve that switches the trap section 11 between a flow system and a closed system.
１０は、トラップされた成分をガスクロマトグラフ部１
２．１３に導入する切換弁である。ガスクロマトグラフ
部１２は、ＰＩＤ検出器２５、ＦＩＤ検出器２６より成
り、ガスクロマトグラフ部１３はＦＩＤ検出器２７から
構成されている。トラップ部上」は、トラップ管１９を
ヒーター２０により捲回し筐体２１内に収納しである。10, the trapped components are transferred to the gas chromatograph section 1
This is a switching valve introduced in 2.13. The gas chromatograph section 12 includes a PID detector 25 and an FID detector 26, and the gas chromatograph section 13 includes an FID detector 27. In the upper part of the trap section, the trap tube 19 is wound by a heater 20 and housed in a casing 21.
筐体２１は切換弁９と又一端に液体窒素容器且に連通し
である、該液体窒素容器２２には隔壁２３を介して窒素
ガス供給管２４を連通させである。The housing 21 communicates with the switching valve 9 and a liquid nitrogen container at one end, and a nitrogen gas supply pipe 24 communicates with the liquid nitrogen container 22 through a partition wall 23.
この反応炉７から送出される反応生成物または、標準ガ
スがトラップされガスクロマトグラフ部１２．１３に導
入されるまでの流れを説明すると、切換弁９．ｌＯは、
初めに黒線の状態（図示）になっている、この時、トラ
ップ部上」は液体窒素容器且から導入された液体窒素で
極低温まで冷やされている。The flow of the reaction product or standard gas sent out from the reactor 7 until it is trapped and introduced into the gas chromatograph section 12.13 will be explained as follows. lO is
Initially, it is in the black line state (shown in the figure), and at this time, the top of the trap section is being cooled to an extremely low temperature by liquid nitrogen introduced from the liquid nitrogen container.
この状態で、反応生成物または、標準ガスがトラップ部
上ユに導入されると、そのトラップ管１９に捕集される
。水素成分は液体窒素の沸点では捕集できないのでその
ままま流されガスクロマトグラフ部１２のＰＩＤ検出器
２５によって分析される。In this state, when a reaction product or a standard gas is introduced into the upper trap section, it is collected in the trap pipe 19. Since the hydrogen component cannot be collected at the boiling point of liquid nitrogen, it is simply flowed away and analyzed by the PID detector 25 of the gas chromatograph section 12.
次の段階として、切換弁９を白線の状態（図示）に切り
換へてトラップ部上」を密閉系にし、液体窒素の導入を
停止し、トラップ部上」内のトラップ管１９に巻いであ
るヒーター２０に通電して、所定の温度まで加熱し、捕
集されていた成分を脱着させる。次に、切換弁ｌＯを白
線の状態（図示）にした後、切換弁９を黒線の状態（図
示）にすることによって、捕集されていた反応生成物ま
たは、標準ガスをガスクロマトグラフ部１２エユ」に導
入する。As the next step, the switching valve 9 is switched to the state shown by the white line (as shown in the figure) to make the upper part of the trap a closed system, the introduction of liquid nitrogen is stopped, and the liquid nitrogen is wound around the trap pipe 19 in the upper part of the trap part. The heater 20 is energized and heated to a predetermined temperature to desorb the trapped components. Next, after setting the switching valve IO to the white line state (shown in the figure), and then setting the switching valve 9 to the black line state (shown in the figure), the collected reaction products or standard gas are transferred to the gas chromatograph section 12. Introduced to "Eyu".
液体窒素の供給は、外部の電磁弁を介して窒素ガス供給
管２４により窒素ガスを液体窒素容器ｌλ内に送り込み
、該容器ｌλ内を加圧することによって、液体窒素をト
ラップ部上」に送出している。To supply liquid nitrogen, nitrogen gas is fed into the liquid nitrogen container lλ through the nitrogen gas supply pipe 24 via an external solenoid valve, and by pressurizing the inside of the container lλ, the liquid nitrogen is sent onto the trap section. ing.
へ）発明の効果
上記の如き本発明によれば、気体又は液体材料を反応装
置により触媒反応させ、反応生成部分を液体窒素を用い
たトラップに導入し、水素部分はスルーさせて他の部分
は捕集した後加熱脱着し、夫々ガスクロマトグラフ部に
導くので、無機ガス、低級炭化水素、測定用のバツクド
カラム、高沸点炭化水素測定用の液相化学結合型フユー
ズドシリ力キャピラリー力ラムの組合せ、バンド巾の縮
少を為しうるコールドトラップの採用により、触媒反応
の結果１分解生成された試料はトラップ部の通過により
Ｈ２は通過させ、炭化水素系は捕集し加熱脱着により夫
々ガスクロマトグラフに導かれ、１回のサンプリングで
Ｈ２，Ｃ１〜Ｃ１５の成分を１回で分析出来、然も、測
定成分の分析はＨ２、ＣＩ −Ｃ１５に限定されず、カ
ラム交換により他成分の分析も可能であり更に、高分離
能、高精度分析を実現できる。f) Effects of the Invention According to the present invention as described above, a gaseous or liquid material is subjected to a catalytic reaction using a reaction device, and the reaction product part is introduced into a trap using liquid nitrogen, the hydrogen part is allowed to pass through, and the other part is After being collected, it is heated and desorbed and guided to the gas chromatograph section, so it is a combination of a back column for measuring inorganic gases, lower hydrocarbons, and a liquid phase chemically bonded fused silica capillary column for measuring high boiling point hydrocarbons. By adopting a cold trap that can reduce the band width, the sample decomposed as a result of the catalytic reaction passes through the trap section, allowing H2 to pass through, and hydrocarbons are collected and transferred to a gas chromatograph by thermal desorption. It is possible to analyze H2, C1 to C15 components in one sampling, but the analysis of the measured components is not limited to H2 and CI-C15, and it is also possible to analyze other components by replacing the column. Furthermore, high resolution and high precision analysis can be achieved.
又各部の制御は自動的に行なわれ、切換弁、オートサン
プラー等により、ガス体試料、液体試料を任意に供給で
き、従ってシーケンスコントロール等により、装置全体
の自動化が為しうることになり、省略化が達成できたIn addition, each part is automatically controlled, and gas samples and liquid samples can be supplied as desired using switching valves, autosamplers, etc. Therefore, the entire device can be automated by sequence control, etc., and omitted. was achieved.
図は本発明一実施例概略説明図である。
１・・・・・・ 切換弁
２・・・・・・ サーマルマスフローコントローラー３
・・・・・・ 切換弁 ４・・・・・・ 検量管
５・・・・・・ オートサンプラー
６・・・・・・ 注入部 ７・・・・・・ 反応
炉８．９．１０・・・・・・切換弁
上」・・・・・・ トラップ部
１２、二・・・・・・ ガるクロマトグラフ１４・・
・・・・ 切換弁 １５・・・・・・ 検量管１６
．１７．１８・・・・・・ボート
１９・・・・・・ トラップ管 ２０・−・・−・ ヒ
ーター２１・・・・・・ 筐体 １」・・・・・・
液体窒素容器２３・・・・・・ 隔壁
２４・・・・・・ 窒素ガス供給管
２５・・・・・・ ＰＩＤ検出器
２６．２７・・・・・・ＦＤＩ検出器
特許出願人 日製ソフトウェア株式会社ガスクロ工業株
式会社The figure is a schematic explanatory diagram of an embodiment of the present invention. 1... Switching valve 2... Thermal mass flow controller 3
...... Selector valve 4... Calibration tube 5... Auto sampler 6... Injection part 7... Reactor 8.9.10. ...On the switching valve... Trap section 12, 2... Gall chromatograph 14...
...... Selector valve 15... Calibration tube 16
．． 17.18... Boat 19... Trap pipe 20... Heater 21... Housing 1''...
Liquid nitrogen container 23... Partition wall 24... Nitrogen gas supply pipe 25... PID detector 26.27... FDI detector patent applicant Nissei Software Gascro Industries Co., Ltd.
Claims (1)
反応生成部分を液体窒素を用いたトラップに導入し、水
素部分はスルーさせて他の部分は捕集した後加熱脱着し
、夫々ガスクロマトグラフ部に導くことを特徴とする触
媒自動試験方法。 ２）サンプリング装置にパルス反応装置を連通させ、切
換弁を介して液体窒素容器及びヒーターを備えたトラッ
プに接続し、該トラップには所望の検出器を連通したこ
とを特徴とする触媒自動試験装置。[Claims] 1) catalytically reacting a gas or liquid material with a reaction device;
An automatic catalyst testing method characterized by introducing the reaction product into a trap using liquid nitrogen, allowing the hydrogen part to pass through, and collecting the other parts, thermally desorbing them, and guiding each part to a gas chromatograph section. 2) A catalyst automatic testing device characterized in that a pulse reaction device is connected to a sampling device, which is connected via a switching valve to a trap equipped with a liquid nitrogen container and a heater, and a desired detector is connected to the trap. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61067790A JPH0718858B2 (en) | 1986-03-26 | 1986-03-26 | Catalyst automatic test equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61067790A JPH0718858B2 (en) | 1986-03-26 | 1986-03-26 | Catalyst automatic test equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62223669A true JPS62223669A (en) | 1987-10-01 |
| JPH0718858B2 JPH0718858B2 (en) | 1995-03-06 |
Family
ID=13355098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61067790A Expired - Lifetime JPH0718858B2 (en) | 1986-03-26 | 1986-03-26 | Catalyst automatic test equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0718858B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999060396A1 (en) * | 1998-05-15 | 1999-11-25 | Fortum Oil And Gas Oy | Arrangement, equipment and method for testing heterogeneous catalysts for short contact time reactions |
| JP2014035275A (en) * | 2012-08-09 | 2014-02-24 | Shimadzu Corp | Gas chromatograph |
| JP2015194456A (en) * | 2014-03-26 | 2015-11-05 | フロンティア・ラボ株式会社 | Gas-phase component analyzer |
| CN114113428A (en) * | 2021-11-12 | 2022-03-01 | 云南电网有限责任公司电力科学研究院 | Device and method for testing liquid organic hydrogen storage material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6144357A (en) * | 1984-08-07 | 1986-03-04 | Idemitsu Kosan Co Ltd | System for testing catalytic activity |
| JPS61204561A (en) * | 1985-03-08 | 1986-09-10 | Jgc Corp | Evaluating method for catalyst activity in fcc and reactivity of raw material |
| JPS62126769U (en) * | 1986-02-03 | 1987-08-11 |
-
1986
- 1986-03-26 JP JP61067790A patent/JPH0718858B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6144357A (en) * | 1984-08-07 | 1986-03-04 | Idemitsu Kosan Co Ltd | System for testing catalytic activity |
| JPS61204561A (en) * | 1985-03-08 | 1986-09-10 | Jgc Corp | Evaluating method for catalyst activity in fcc and reactivity of raw material |
| JPS62126769U (en) * | 1986-02-03 | 1987-08-11 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999060396A1 (en) * | 1998-05-15 | 1999-11-25 | Fortum Oil And Gas Oy | Arrangement, equipment and method for testing heterogeneous catalysts for short contact time reactions |
| JP2014035275A (en) * | 2012-08-09 | 2014-02-24 | Shimadzu Corp | Gas chromatograph |
| JP2015194456A (en) * | 2014-03-26 | 2015-11-05 | フロンティア・ラボ株式会社 | Gas-phase component analyzer |
| CN114113428A (en) * | 2021-11-12 | 2022-03-01 | 云南电网有限责任公司电力科学研究院 | Device and method for testing liquid organic hydrogen storage material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0718858B2 (en) | 1995-03-06 |
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