JPH0718858B2 - Catalyst automatic test equipment - Google Patents

Description

TECHNICAL FIELD The present invention relates to an automatic catalyst test method and apparatus, and is for automatically performing performance, test, and evaluation of reactivity, durability, etc. of an industrial catalyst. It is a thing.

(B) Conventional technology As a catalyst test device, a flow reactor and a device using a pulse reaction part are used, but since they are used independently, a wide range of component analysis such as H2, C1-C15 component analysis is possible. To do this, one sampling is not enough and many times are required.

C) Problems to be solved For this reason, a large amount of sample is required, and it takes time and time for analysis, and it is not possible to arbitrarily measure a gas sample or liquid sample, and continuous automatic analysis cannot be performed. Furthermore, high resolution analysis was not possible.

D) Means for solving the problem A packed column (for measurement of H2, C1 to C3) and a liquid phase chemically-bonded fused silica capillary column (for measurement of C4 to C15) can be combined, and a cold trap is adopted. The H2 and C1 to C15 components can be analyzed at a single time by the above-mentioned method, and the analysis of measured components is not limited to H2 and C1 to C15, and other components can be analyzed by column exchange. Then, the reaction product part obtained by catalytically reacting the gas or liquid material by the catalytic reaction device is introduced into the trap using liquid nitrogen, the hydrogen part is allowed to pass through, and the other part is collected and then desorbed by heating, and each is subjected to gas chromatography. In the automatic catalyst testing device that leads to the reactor, the sampling device is connected to the injection part having the vaporizing function and the pulse reaction device, and a trap equipped with a liquid nitrogen container and a heater is provided through a switching valve. Connected to, the said trap portion, characterized in that selectively communicating the desired detector.

E) Example 1 is a switching valve for switching between air used for catalyst regeneration and He used for actual reaction analysis, and 2 is a thermal mass flow controller for controlling the flow rate of the fluid. Of course, the thermal mass flow controller 2 can set the flow rate from the outside. Reference numeral 3 is a switching valve that sends the gas sample to the injection unit 6. The switching valve is connected to the port 16, and a gas sample is flown from the port 16 to fill the calibration tube 4 to switch to the switching valve 3 so that the gas material is sent to the injection portion 6.

An autosampler 5 is configured to automatically deliver a fixed amount of liquid sample to the injection unit 6. The injection part 6 has a function of vaporizing the liquid sample.

Reference numeral 7 is a reaction furnace in which the catalyst is loaded in a quartz reaction tube and inserted therein. The reaction furnace 7 can change the set temperature from the outside, and a pulse reaction furnace is preferably used.

A switching valve 8 has a function of switching between the case where the actual reaction components are sent to the trap section 4 and the case where the processing gas flowing from the reaction furnace at the time of catalyst regeneration is sent to the outside of the system. In the latter case, the standard gas can be introduced into the trap section 11 by the switching valve 14 when creating the calibration curves for the gas chromatograph sections 12 and 13. In this case, the standard gas is made to flow from the port 17 to fill the calibration curve 15 and the switching valve 14 is switched.

Reference numeral 9 is a switching valve for switching the trap portion 11 to a flow system or a closed system.

10 is a gas chromatograph section 12 for trapped components,
It is a switching valve introduced in 13. Gas chromatograph section 12
Is composed of a PID detector 25 and an FID detector 26, and the gas chromatograph unit 13 is composed of an FID detector 27. The trap section 11 has a casing in which a trap tube 19 is wound by a heater 20.
It is stored in 21. The housing 21 is connected to the switching valve 9 and also to the liquid nitrogen container 22 at one end. The liquid nitrogen container 22 has a partition wall.
A nitrogen gas supply pipe 24 is connected via 23.

Explaining the flow until the reaction product sent from the reaction furnace 7 or the standard gas is introduced into the trapped gas chromatograph sections 12 and 13, the switching valves 9 and 10 are initially in a black line state ( (Shown). At this time, the trap section 11 is cooled to an extremely low temperature by the liquid nitrogen introduced from the liquid nitrogen container 22 . In this state, the reaction product or
When the standard gas is introduced into the trap section 11 , it is collected in the trap tube 19. Since the hydrogen component cannot be repaired at the boiling point of liquid nitrogen, it is flowed as it is and the gas chromatograph section 12
Analyzed by PID detector 25.

As a next step, the trap portion 11 to switch the switch valve 9 to the state of the white line (shown) to a closed system, a heater 20 for the introduction of liquid nitrogen was stopped, it is wound in a trap tube 19 in the trap unit 11 Is energized and heated to a predetermined temperature to desorb the collected components. Next, the changeover valve 10 is set to the white line state (illustrated), and then the changeover valve 9 is set to the black line state (illustrated), so that the collected reaction product or standard gas is removed from the gas chromatograph section 12 , 13 to be introduced.

The liquid nitrogen is supplied by sending nitrogen gas into the liquid nitrogen container 22 through the nitrogen gas supply pipe 24 via an external solenoid valve, and pressurizing the inside of the container 22 , thereby sending the liquid nitrogen to the trap portion 11. There is.

F) Effects of the Invention According to the present invention as described above, a gas or liquid material is catalytically reacted by a reaction device, a reaction product part is introduced into a trap using liquid nitrogen, a hydrogen part is passed through, and other parts are In an automatic catalyst testing device that collects and then desorbs heat and guides them to the gas chromatograph part, the sampling device is connected to the injection part having a vaporization function and the pulse reaction device, and the liquid nitrogen container and heater are connected through a switching valve. Since a desired detector was selectively communicated with the trap section equipped with, the inorganic gas, lower hydrocarbon, packed column for measurement, liquid phase chemical bond for high boiling point hydrocarbon measurement Type fused silica capillary column combination,
By adopting a cold trap that can reduce the band width, the sample that has been decomposed as a result of the catalytic reaction is passed through the trap part to pass H2, the hydrocarbon system is collected and heated and desorbed into gas chromatographs. It is possible to analyze the components of H2 and C1 to C15 with one sampling, and the analysis of the measured components is not limited to H2 and C1 to C15, and other components can be analyzed by column exchange. Furthermore, high resolution and high precision analysis can be realized.

In addition, the control of each part is performed automatically, and the gas sample and the liquid sample can be arbitrarily supplied by the switching valve, the auto sampler, etc. Therefore, the sequence control etc. can automate the entire device, and thus it is omitted. Was achieved.

[Brief description of drawings]

FIG. 1 is a schematic explanatory view of an embodiment of the present invention. 1 ... Switching valve 2 ... Thermal mass flow controller 3 ... Switching valve, 4 ... Weighing tube 5 ... Auto sampler 6 ... Injection part, 7 ... Reactor 8, 9, 10 ... Switching valve 11 ... Trap unit 12 , 13 ...... Gas chromatograph 14 …… Switching valve, 15 …… Calibration tube 16,17,18 …… Port 19 …… Trap tube, 20 …… Heater 21 …… Case, 22 …… Liquid nitrogen container 23 …… Partition 24 …… Nitrogen gas supply pipe 25 …… PID detector 26, 27 …… FDI detector

Claims (1)

[Claims] 1. A gas or liquid material is catalytically reacted by a reaction device, a reaction-produced portion is introduced into a trap using liquid nitrogen, a hydrogen portion is passed through, and the other portion is collected and then desorbed by heating. In an automatic catalyst test device that leads to a gas chromatograph unit, the sampling unit is connected to an injection unit having a vaporization function and a pulse reactor, and is connected to a trap unit equipped with a liquid nitrogen container and a heater through a switching valve, An automatic catalyst testing device, wherein a desired detector is selectively communicated with the trap portion.