JPH07294395A - Rapid gas sampler - Google Patents

Abstract

PURPOSE:To provide a rapid gas sampler which is effective for monitoring the reaction phenomenon or behavior in a process by sampling an adsorption reaction high-temperature gas generated from the process. CONSTITUTION:The gas sampler consists of stainless steel large-capacity Gas cylinder Groups b1-b15, rotary pumps 7 and 10 for sucking and discharging gas, a sheet heater 11 and a current power supply 12 for heater which are wound around the cylinder groups b1-b15 for heating and preserving temperature, and a sequence control circuit 15 for controlling electro-magnetic switching valves V1-V18 of all gas paths and the rotary pumps 7 and 10 which are connected in parallel for storing an adsorption reaction high-temperature gas generated from a process quickly and regularly, thus obtaining a simple and inexpensive the gas sampler where the suction can be ignored.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention collects adsorption-reactive high temperature gas, for example, SO ₂ and H ₂ S, from a process in a short period of time and regularly, and analyzes various reactions and reductions in the process. -It relates to a rapid gas sampler for process suitable for grasping.

[0002]

2. Description of the Related Art Generally, by analyzing gas components generated from various processes and analyzing and grasping reactions and reductions during heating and combustion in the processes, process optimization control and its operation state are performed. The maintenance and monitoring of gas is often done, but at this time, a gas sampler suitable for the purpose is required.

FIG. 2 shows a schematic view of an example of a conventional gas sampler. These gas samplers are made of glass, metal, polymer material pipes, etc., (a) is a glass syringe type, (b) is a gas sampling container with open / close valves at both ends, the former, The gas is manually sucked into the cylinder 1 of the syringe, and the latter uses the on-off valves 2 and 2'to take the sample gas into the gas sampling container 3 by the exhaust pressure from the process, and the other. There is a case where the rotary pump 4 for suction is connected to and the sample gas is taken into the gas sampling container 3. At this time, when it is necessary to hold the gas at a predetermined temperature or higher until it is introduced into the gas analyzer, such as an adsorption-reactive high temperature gas, the gas sampling container 3 may be held in a small thermostat after sampling the sample gas. .

Such a conventional general-purpose gas sampler is described in "Introduction Gas Chromatography, May 1978, Nankodo Co., Ltd., P33-P36", and many similar documents are known. is there. these,
The sample gas collected by the gas sampler is usually several ml.
~ Several hundred ml, gas analyzer to several ml ~ tens of ml
The following is introduced manually or automatically, and the required gas component is analyzed within an analysis time (analysis cycle) of about several minutes to several tens of minutes, though it varies depending on the gas component to be analyzed and the number of components.

Therefore, it cannot be applied to the purpose of regularly collecting the adsorption-reactive high-temperature gas from the process aimed at by the present invention within a short time of several tens of seconds to several minutes. In addition, since the sampling volume is small, the amount of gas adsorbed in the gas sampler cannot be ignored even if the sample is held in a thermostatic chamber until it is introduced into the gas analyzer. It is also effective to increase the size of the gas sampling container 3 (including the use of a high-pressure gas cylinder) in order to reduce the influence of adsorption. However, the size of the thermostat becomes larger accordingly, and it is practical in terms of installation space and price. The problem is extremely large.

[0006]

DISCLOSURE OF THE INVENTION The present invention is generated by heating / combusting a charge in a process, and the time from the start to the end of the generation is very short for several tens of seconds to several minutes. Another object of the present invention is to provide a gas sampler capable of analyzing and ascertaining various reactions and phenomena in the process by collecting a high-temperature gas having a strong adsorptive reactivity in which the generated gas component in the short time changes with time. In other words, the sample gas is sampled at regular time intervals within an arbitrary short time, and the batch-type analysis processing is possible regardless of the analysis time (analysis cycle) of the gas analyzer. Another object of the present invention is to provide a compact, simple, and inexpensive gas sampler in which the amount of gas adsorbed in the gas sampling container, which is difficult to achieve with the conventional gas sampler, can be suppressed to a negligible amount in analysis.

[0007]

In order to solve the above problems, as shown in FIG. 1, the adsorption reactivity which is generated within a short time by heating and burning the charge in the process 5 and which changes with time Assuming that the stored gas pressure is close to normal pressure, cut out a thin hot-corrosion-resistant stainless steel inner surface polishing pipe to the required length, seal both ends, and connect a sample gas conduit to open and close the strong gas large gas cylinder b ₁ ~b ₁₅ provided with the valve _{V 2, V '2 ~V 16} , V' 16 connected in parallel with a large-capacity gas cylinder group, sequentially for each sampling time of the sample gas, by switching the gas bottle The method of taking in was adopted.

Further, the sheet heater 11 was wound around the gas cylinder, sample gas conduit, etc., and the temperature of the sample gas to be sampled was monitored and kept at a predetermined temperature. Further, an opening / closing valve V ₁ is provided at the inlet / outlet side of the gas cylinder or sample gas conduit path.
~ V ₁₈ and on-off three-way valve V ₁₇ are provided, and the on-off valve and suction /
The suction rotary pumps 7 and 10 were controlled by the sequence control circuit 15 to totally control sample gas collection and introduction into the gas analyzer 8.

That is, the gist of the present invention is as follows. A large-capacity group of gas cylinders connected in parallel for storing the high temperature gas produced by the adsorption reaction from the process in a short time and regularly, a rotary pump for sucking and sucking the gas into and from the cylinder group, and from the process A sheet heater for winding and heating the cylinder group and sample gas conduit leading to the gas analyzer, a power source for the heater, a heating temperature controller, an on-off valve, and a sequence control circuit for a rotary pump. It is a rapid gas sampler characterized by consisting of. The capacity of the gas cylinder is several liters to several tens of liters.
And The on-off valve may be manually operated, but may be an electromagnetic on-off valve.

[0010]

The operation of the present invention will be described in detail below. In the present invention, the opening and closing valve V ₁ ~V ₁₈ which is controlled gas generated from the process 5 in the sequence control circuit 15, closing the three-way valve V ₁₇ and, by the operation of the suction-suction rotary pump 7 and 10, connected in parallel Since the selected large-capacity gas cylinders b _{1 to} b ₁₅ are sequentially switched and taken in, the sample gas can be sampled at an arbitrary short time and at regular intervals. In addition, by collecting the sample gas in the gas cylinder and keeping it warm, the amount of gas adsorbed during storage can be suppressed to a level that can be ignored in analysis,
Batch analysis processing can be performed within a predetermined analysis time of the gas analyzer 8.

Further, the large-capacity gas cylinders b _{1 to} b ₁₅ are manufactured by using thin-walled corrosion-resistant stainless steel inner surface polishing tubes, and the large-capacity gas cylinder groups which are normally kept warm by using a constant temperature bath are respectively formed into sheets. By winding the heater 11 to heat and keep it warm, etc., it is possible to construct a compact, simple, and inexpensive process large-volume gas sampler with a constant temperature function.

[0012]

Embodiments of the present invention will be described below in detail with reference to a case where an electromagnetic opening / closing valve is used as an opening / closing valve. Figure 1
FIG. 1 shows a schematic block diagram of a rapid high capacity gas sampler for a process according to the present invention. The gas sampler is a process 5
An electromagnetic on-off valve V ₁ is provided at the sampling port 6 for generating the gas, and large-capacity gas cylinders b _{1 to} b ₁₅ for storing the generated gas are connected in parallel to form a large-capacity gas cylinder group, and the generated gas is sucked and sucked into the gas cylinder. solenoid valve V ₂ for, V _'2 ~
V ₁₆ and V ′ ₁₆ , the rotary pump 7, the electromagnetic open / close valve V17 for switching the sample gas path provided between the large-capacity gas cylinder group and the gas analyzer 8, the dust of the sample gas introduced into the gas analyzer 8, and the like. Filters 9 and 9'for removing water
And a rotary pump 10 for introducing the sample gas into the gas analyzer 8, and a sample gas conduit extending from the process 5 to the gas analyzer 8, the gas cylinder group, and the electromagnetic opening / closing valve are wound to heat and keep heat. Seat heater 11, power source 12 for the heater, and thermocouple 13 provided in each gas cylinder
Power supply for seat heater by detecting the temperature of
2, a heating temperature controller 14 for controlling the electric current, the electromagnetic on-off valves V _{1 to} V ₁₈ , the electromagnetic on-off three-way valve V _17, and the rotary pumps 7, 1.
And a sequence control circuit 15 for controlling 0. In addition, in order to prevent heat dissipation of the gas cylinder group, the outer surface of the seat heater 11 was entirely covered with a heat insulating material.

First, the sequence control circuit 15 sets the opening / closing of each of the electromagnetic opening / closing valves V _{1 to} V ₁₈ and the electromagnetic opening / closing three-way valve V ₁₇ of the entire gas sampler, and the driving timing of the rotary pumps 7 and 10. In addition, the sample gas introduction path, each electromagnetic opening / closing valve, the large-capacity gas cylinder group, and the like are connected to the electric current of the seat heater power source 12 controlled by the heating temperature controller 14 several hours before the start of the operation of the process 5 and each portion. It is heated and held in advance at a predetermined temperature according to the temperature detected by the attached thermocouple. After a lapse of a predetermined time from the start of operation of the process 5, the generated process gas is the electromagnetic on-off valves V ₁ and V of the sample gas conduit connected to the gas sampling port 6.
₂ , V ′ ₂ and the electromagnetic opening / closing three-way valve V ₁₇ are opened, the rotary pump 7 is driven at the same time, and a predetermined amount of the sample gas is sucked into the large-capacity gas cylinder b ₁ through the filter 9. valve V _2, V _'2 is closed. Next, the gas cylinder b ₂ close valve V _3, V 'and ₃ opens, the large-capacity gas cylinder b ₂ After the sample gas has been sucked by a predetermined amount, the solenoid valve V _3, V' ₃ is closed. Thereafter, similarly, the sample gas is repeatedly collected in each gas cylinder, and when the collection is completed, the electromagnetic on-off valves V ₁ and V ₁₇ are closed and the rotary pump 7 is stopped.

The gas collected from each of the gas cylinders can be analyzed in batches for the required gas components in the gas analyzer 8 after a short time has elapsed. The procedure is
First, the residual gas in the gas conduit from the gas cylinder group outlet to the gas analyzer 8 is opened by opening the electromagnetic opening / closing three-way valve V ₁₇ , and
After the rotary pump 7 is driven and exhausted, the electromagnetic on-off valves V ′ ₂ and V ₁₈ are opened, and the electromagnetic on-off three-way valve V ₁₇ is switched. At the same time, the rotary pump 10 is driven and the sample gas is fed to the gas analyzer 8. after There has been introduced, the solenoid valve V _'2, V ₁₈
Is closed, the rotary pump 10 is stopped, and a required gas component is analyzed at a predetermined analysis time.

Next, again, the residual gas in the gas conduit extending from the gas cylinder outlet side to the gas analyzer 8 is switched over by the electromagnetic open / close three-way valve V ₁₇ and the rotary pump 7 is driven to be exhausted. The valves V ′ ₃ and V ₁₈ are opened, and the electromagnetic opening / closing three-way valve V ₁₇ is switched. At the same time, the rotary pump 10 is driven to introduce the sample gas into the gas analyzer 8, and the electromagnetic opening / closing valve V ′ ₃ is closed and rotated. The pump 10 is stopped, and the required gas component is analyzed in the specified analysis time. After that, the analysis of the collected gas of each gas cylinder is repeatedly performed in the same order as described above, and the fluctuation of the gas components generated from the process 5 and the generation / reaction phenomenon can be analyzed to obtain an evaluable analysis result.

In the present invention shown in FIG. 1, a rotary kiln was used as the process 5, and the contents thereof at the time of various uses, the scrap material scraped into small pieces with the coating material and the polymer thin film adhered thereto were used as the charging material. Further, a large-capacity gas cylinder b ₁ of the rapid large-capacity gas sampler according to the present invention shown in FIG.
A gas capacity of 10 liters / tube was used for each of -b ₁₅ and ₁₅ tubes were collectively arranged in two rows to form a large capacity gas cylinder group. The gas cylinder group by the sheet heater 11 was held at 110 ° C. by the heating temperature controller 14.
The rotary pumps 7 and 10 used had an exhaust capacity of 30 liters / min and 1.0 liters / min, respectively.

FIG. 3 shows a schematic cross-sectional view of the operating state of the rotary kiln. In operation, the rotary kiln 16 burns coke oven gas in the gas burner 18 while rotating at a low speed by the tilting / rotating mechanism 17 in advance, preheats the inside of the kiln 16, and then loads the scrap material 20 from the charging port 19. The scrap material 20 is heated while moving in the kiln 16 toward the discharge port 21, and various surface deposits are burned. The gas generated in this process is the exhaust port 2
2 and is discharged from the gas sampling port 6 by opening the electromagnetic on-off valve V ₁ . Further, the scrap material 20 in which the surface deposits are burned is discharged from the discharge port 21.

The exhaust gas from the rotary kiln 16 is
A maximum of 600 ° C is reached. After starting combustion of this exhaust gas, 1
At intervals of 15 minutes, 15 large-capacity gas cylinders b ₁ to b ₁₅ are sequentially automatically sucked and stored, and after combustion is completed, the first generated gas is sampled from the cylinders b ₁ to b _{15 in a} 5-minute cycle. A sample gas was introduced into the gas analyzer 8 (general-purpose gas chromatograph), and H ₂ , CO, CO ₂ , and H _{2 were} added as gas components.
Five components of S and SO ₂ were analyzed.

FIG. 4 shows a typical example of the result of analyzing the gas components generated in the rotary kiln using the rapid large-capacity gas sampler according to the present invention. The vertical axis represents the generated gas concentration, and the horizontal axis represents the elapsed time after charging the scrap material. From this figure, from the surface deposits of the scrap material 20 which is heated and burned in the rotary kiln 16, H ₂ S gas having strong adsorption reactivity is rapidly generated / increased about 6 minutes after the start of charging,
On the other hand, it can be clearly understood that the S0 ₂ gas gradually increases, reaches the maximum in about 10 to 12 minutes, and then rapidly decreases. Further, from the results, when the rapid large-capacity gas sampler according to the present invention is applied, the analysis value of the high-temperature gas having strong adsorption reactivity is improved by about 10 times as compared with the case where the conventional gas sampler is used, and the analysis is performed. It was found that the accuracy and reproducibility are greatly improved, and they serve as important guidelines for controlling and stabilizing the operation.

Although the rotary kiln is used as the process and the gas sampler for monitoring the time change of the gas component generated in the heating and burning process of the scrap material is described here, the process is not limited to the rotary kiln. The effect does not change even if the type or temperature of the generated / exhaust gas changes. In addition, the capacity of the gas cylinder and the increase or decrease in the number of cylinders are not restricted. Further, since it is possible to accurately grasp the behaviors of generation / reaction in the process, exhaust gas, etc. associated with heating / combustion, it can be effectively applied to various process control and process behavior monitoring.

[0021]

As described below, according to the present invention, a large amount of adsorption-reactive high-temperature gas generated from the process can be regularly collected in an arbitrary time, and the collection and storage can be performed. Since the amount of sample gas adsorbed in the sample is suppressed to a negligible amount in analysis, it is possible to accurately analyze the changing process of high-temperature gas components with strong adsorption reactivity, which is extremely effective in practice, simple, and inexpensive with a constant temperature function. A rapid large volume gas sampler for the process is obtained.

[Brief description of drawings]

FIG. 1 is an explanatory diagram of a device configuration of a rapid large-capacity gas sampler according to the present invention.

FIG. 2 shows a schematic diagram of an example of a conventional gas sampler.

FIG. 3 is a schematic cross-sectional explanatory diagram of an operating state of a rotary kiln.

FIG. 4 is an explanatory diagram showing a typical example of the result of analysis of gas components generated in a rotary kiln using the rapid large-capacity gas sampler according to the present invention.

[Explanation of symbols]

1 Cylinder 2 2'Open / close valve 3 Gas sampling container 4 Inhalation rotary pump 5 Process 6 Gas sampling port 7 Rotary pump 8 Gas analyzer 9 and 9'filter 10 Rotary pump 11 Seat heater 12 Power source for seat heater 13 Thermocouple 14 heating temperature controller 15 sequence controller 16 rotary kiln 17 tilting and rotating mechanism 18 gas burner 19 spout 20 scrap material 21 outlet 22 outlet b ₁ ~b ₁₅ mass gas cylinder V ₁ ~V _16, V ₁₈ solenoid valves V ₁₇ Solenoid on-off valve

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[Procedure amendment]

[Submission date] June 3, 1994

[Procedure Amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0001

[Correction method] Change

[Correction content]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention collects adsorption-reactive high-temperature gas such as SO ₂ and H ₂ S from a process in a short period of time and regularly, and analyzes various reactions and phenomena in the process. -It relates to a rapid gas sampler for process suitable for grasping.

[Procedure Amendment 2]

[Document name to be amended] Statement

[Name of item to be corrected] 0002

[Correction method] Change

[Correction content]

[0002]

2. Description of the Related Art Generally, gas components generated from various processes are analyzed to detect the reaction during heating and combustion in the process.
By analyzing and understanding the response and phenomena , process optimization control and maintenance / monitoring of its operating state are often performed, but in this case, a gas sampler suitable for the purpose is required.

[Procedure 3]

[Document name to be amended] Statement

[Correction target item name] 0009

[Correction method] Change

[Correction content]

That is, the gist of the present invention is as follows. A group of large-capacity gas cylinders connected in parallel for storing the adsorption-reactive high-temperature gas generated from the process in a short time and regularly, a rotary pump for sucking and sucking gas into and from the cylinder group, and from the process A sheet heater for winding and heating the cylinder group and sample gas conduit leading to the gas analyzer, a power source for the heater, a heating temperature controller, an on-off valve, and a sequence control circuit for a rotary pump. It is a rapid gas sampler characterized by consisting of. The capacity of the gas cylinder is several |
And The on-off valve may be manually operated, but may be an electromagnetic on-off valve.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0012

[Correction method] Change

[Correction content]

[0012]

Embodiments of the present invention will be described below in detail with reference to a case where an electromagnetic opening / closing valve is used as an opening / closing valve. Figure 1
FIG. 1 shows a schematic block diagram of a rapid high capacity gas sampler for process according to the present invention. The gas sampler is a process 5
An electromagnetic opening / closing valve V ₁ is provided at the generated gas sampling port 6 of the above, and large-capacity gas cylinders b _{1 to} b ₁₅ for storing the generated gas are connected in parallel to form a large-capacity gas cylinder group, and the generated gas is sucked and sucked out. solenoid valve _V 2 for, V _'2 ~V
₁₆ , V ′ ₁₆ , a rotary pump 7, a three-way valve V ₁₇ for switching the sample gas path provided between the large-capacity gas cylinder group and the gas analyzer 8, dust of the sample gas introduced into the gas analyzer 8, and the like. A filter 9 for removing water,
9 ', a rotary pump 10 for introducing the sample gas into the gas analyzer 8, a sample gas conduit extending from the process 5 to the gas analyzer 8, the gas cylinder group, and a winding coil for heating and keeping the electromagnetic on-off valve. A seat heater 11, a heater power supply 12, a thermocouple 13 provided in each gas cylinder, a heating temperature controller 14 for detecting the temperature of the thermocouple and controlling the current of the seat heater power supply 12, and The electromagnetic on-off valves V _{1 to} V ₁₈ , the electromagnetic on-off three-way valve V _17, and the sequence control circuit 15 for controlling the rotary pumps 7 and 10. In addition, in order to prevent heat dissipation of the gas cylinder group, the outer surface of the seat heater 11 was entirely covered with a heat insulating material.

[Procedure Amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0013

[Correction method] Change

[Correction content]

First, the sequence control circuit 15 sets the opening and closing of the electromagnetic on-off valves V _{1 to} V ₁₈ , the electromagnetic on-off three-way valve V ₁₇ , and the drive timing of the rotary pumps 7 and 10 of the entire gas sampler. In addition, the sample gas introduction path, each electromagnetic opening / closing valve, the large-capacity gas cylinder group, and the like are connected to the electric current of the seat heater power source 12 controlled by the heating temperature controller 14 several hours before the start of the operation of the process 5 and each portion. It is heated and held in advance at a predetermined temperature according to the temperature detected by the attached thermocouple. After a lapse of a predetermined time from the start of operation of the process 5, the generated process gas is generated by the electromagnetic on-off valves V ₁ , V ₂ , V ′ _{2 of} the sample gas conduit connected to the gas sampling port 6 and the electromagnetic on-off three-way valve V. _{When 17} is opened, the rotary pump 7 is driven at the same time, so that a predetermined amount of the sample gas is sucked into the large-capacity gas cylinder b ₁ through the filter 9, and then the electromagnetic opening / closing valves V ₂ and V ′ ₂ are closed. Next, the solenoid on-off valves V ₃ and V ′ _{3 of the} gas cylinder b ₂
Is opened, and a predetermined amount of the sample gas is sucked into the large-capacity gas cylinder b ₂ , and then the electromagnetic opening / closing valves V ₃ and V ′ ₃ are closed. Hereinafter, similarly, the sample gas is repeatedly collected in each gas cylinder, and when the collection is completed, the electromagnetic on-off valves V ₁ and V ₁₇ are closed and the rotary pump 7 is stopped.

Claims (1)

[Claims] 1. A large-capacity group of gas cylinders connected in parallel for storing the adsorption-reactive high-temperature gas generated from the process in a short time and regularly, and a rotation for sucking and sucking the gas into and from the group of cylinders. A pump, a group of cylinders from the process to the gas analyzer, and a sheet heater for winding and heating the sample gas conduit to heat and keep heat, a power source for the heater, a heating temperature controller, an on-off valve, and a rotation. A rapid gas sampler consisting of a sequence control circuit of a pump.