CN113917056A - Hydrogen flame ionization detector system with ultralow energy consumption and material consumption - Google Patents
Hydrogen flame ionization detector system with ultralow energy consumption and material consumption Download PDFInfo
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Abstract
The invention discloses a hydrogen flame ionization detector system with ultralow energy consumption and material consumption, and belongs to the technical field of gas chromatograph equipment. The detector comprises a detector body, wherein the detector body comprises a base, a nozzle, a collector, a catalytic oxidation reactor and a heat insulation layer, the nozzle and the collector are arranged on the base, the collector is positioned above flame generated by the nozzle, the catalytic oxidation reactor and the base are integrally formed, the catalytic oxidation reactor is positioned on the outer side of the collector, the heat insulation layer is sleeved on the outer sides of the base and the catalytic oxidation reactor, the detector body is used for matching with a heat exchanger and an electrolysis reactor to detect sample gas to be detected, the nozzle and the collector are installed on the base, and the nozzle is used for ejecting flame generated in the combustion process of hydrogen and combustion-supporting gas.
Description
Technical Field
The invention relates to the technical field of gas chromatograph equipment, in particular to a hydrogen flame ionization detector system with ultralow energy consumption and material consumption.
Background
The hydrogen Flame Ionization Detector (FID) is a detector widely applied in the existing gas chromatograph, is used for detecting hydrogen flame ionization, and has the advantages of high sensitivity, low detection limit and the like.
The existing hydrogen flame ionization detector needs hydrogen as fuel gas, except hydrocarbon air as combustion-supporting gas, the cleanliness of fuel gas and combustion-supporting gas has obvious influence on the indexes such as noise and detection limit of the detector, the fuel gas and combustion-supporting gas are mainly provided by two modes at present, one mode is bottled high-pressure gas, and the mode needs frequent replacement and has higher use cost; the other is a gas generator, the hydrocarbon removing air is generally used by an air compressor matched with a hydrocarbon removing system, and the gas generator has larger volume and difficult movement; hydrogen gas is produced by electrolysis, and the pressure of the gas cylinder needs to be paid attention to constantly and the gas cylinder needs to be replaced by adopting the gas cylinder as a gas source; the chromatograph using the air compressor and the hydrocarbon removal system has relatively high energy consumption and occupies more public resources.
And the working temperature of the existing hydrogen flame ionization detector is more than 200 ℃, the detector needs to be continuously heated and is used for heating the detector body, fuel gas and combustion-supporting gas, energy recovery is not carried out on combustion heat, tail gas heat, liquefaction latent heat of product water vapor and the like, the latent heat is directly dissipated in the surrounding environment, the energy consumption of the system is increased, and the portable chromatograph powered by a battery causes higher pressure on the battery.
And the water vapor generated by the combustion of the existing hydrogen flame ionization detector is directly discharged in the air without being recovered, so that the ambient working environment is easily influenced.
Disclosure of Invention
The present invention is directed to a hydrogen flame ionization detector system with ultra-low energy and material consumption to solve the above-mentioned problems of the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: including the detector body, the detector body includes base, nozzle, collector, catalytic oxidation reactor and heat preservation, be provided with nozzle and collector on the base, just the collector is located the flame top that the nozzle produced, catalytic oxidation reactor and base integrated into one piece, just catalytic oxidation reactor is located the collector outside, base and catalytic oxidation reactor outside cover have the heat preservation, and the detector body is used for coordinating heat exchanger and electrolytic reactor to detect the sample gas that awaits measuring, and the base is used for installing nozzle and collector, and the nozzle is arranged in the flame blowout that produces with hydrogen and combustion-supporting gas combustion process, and the collector is arranged in producing ionization signal and receiving in the flame of nozzle spun, and the collector is insulating with the base, avoids having the electric field between the two, produces the influence to the testing result, and catalytic oxidation reactor purifies the combustion-supporting gas after preheating through the catalytic oxidation agent of inside packing, avoid combustion-supporting gas cleanliness factor to hang down and produce showing the influence to indexes such as the noise of detector body and detection limit, reduced the detection effect of detector body, the heat preservation is arranged in reducing the heat loss that produces in the detector body.
Furthermore, a chromatographic column interface is arranged at the bottom of the base, a hydrogen inlet and a combustion-supporting gas inlet are arranged on one side of the base, the combustion-supporting gas inlet is positioned above the hydrogen inlet, a gas outlet is arranged at the top of the base, a heating rod mounting hole and a temperature sensor mounting hole are arranged on one side of the base, the temperature sensor mounting hole is positioned around the heating rod mounting hole, the chromatographic column interface is used for allowing a sample gas to be detected after being separated by a chromatographic column to enter, the hydrogen inlet is used for allowing hydrogen generated after water is electrolyzed by an electrolysis reactor to enter, the combustion-supporting gas inlet is used for allowing combustion-supporting gas purified by a catalytic oxidation reactor to enter, the gas outlet is used for transmitting tail gas generated by combustion in the detector body to a heat exchanger through a pipeline, the heating rod mounting hole is used for mounting a heating rod, and the hydrogen and the combustion-supporting gas injected into the detector body are combusted by heating the mounted heating rod to 250 ℃, the temperature sensor mounting hole is used for mounting a temperature sensor, and the temperature inside the detector body is measured, so that insufficient combustion of hydrogen and combustion-supporting gas is avoided.
Furthermore, the inner cavity of the catalytic oxidation reactor is filled with catalytic oxidant, the outer side of the catalytic oxidation reactor is provided with a combustion-supporting gas inlet II and a combustion-supporting gas outlet, the combustion-supporting gas outlet is connected with the combustion-supporting gas inlet I through a pipeline, the catalytic oxidant is used for purifying combustion-supporting gas injected into the catalytic oxidation reactor, the combustion-supporting gas inlet II is used for enabling combustion-supporting gas preheated by the heat exchanger to enter, the combustion-supporting gas outlet is used for being connected with the combustion-supporting gas inlet I through a pipeline, and the combustion-supporting gas purified by the catalytic oxidant is conveyed to the detector body.
Furthermore, the hydrogen flame ionization detector system also comprises a heat exchanger, a condensed water collector, an electrolysis reactor, a hydrogen precise flow controller, a combustion-supporting gas precise flow controller, a filter and a combustion-supporting gas pump, wherein the heat exchanger is respectively connected with the detector body and the combustion-supporting gas precise flow controller through pipelines, the condensed water collector is installed on the heat exchanger and is connected with the electrolysis reactor through a pipeline, the electrolysis reactor is connected with one end of the hydrogen precise flow controller, which is far away from the detector body, through a pipeline, one end of the hydrogen precise flow controller, which is far away from the electrolysis reactor, is connected with the detector body through a pipeline, one end of the combustion-supporting gas precise flow controller is connected with the heat exchanger through a pipeline, the other end of the combustion-supporting gas precise flow controller is connected with the filter through a pipeline, and one end of the filter, which is far away from the combustion-supporting gas precise flow controller, is connected with the combustion-supporting gas pump through a pipeline, the heat exchanger is used for preheating the injected combustion-supporting gas, discharging low-temperature tail gas to the atmosphere and conveying condensed water generated in the heat exchange process to the condensed water collector, the condensed water collector is used for collecting the condensed water, and the collected condensed water is discharged to an electrolysis reactor, the electrolysis reactor is used for electrolyzing the water source injected from the water replenishing port or the condensed water conveyed from the condensed water collector, and carry the hydrogen that produces after will electrolyzing to the accurate flow controller of hydrogen, the accurate flow controller of hydrogen is used for adjusting the hydrogen volume of pouring into the inside of detector body into, and the accurate flow controller of combustion-supporting gas is used for adjusting the combustion-supporting gas volume of pouring into the inside of heat exchanger into, and the filter is arranged in filtering the water and the fixed granule in the combustion-supporting gas, and the combustion-supporting air pump is used for pressurizeing the combustion-supporting gas of pouring into to the external world, guarantees that the combustion-supporting gas volume of pouring into is enough to react with hydrogen.
Furthermore, a heat exchange fin is arranged in the heat exchanger, a cold medium inlet, a cold medium outlet, a heat medium inlet and a heat medium outlet are arranged on the outer side of the heat exchanger, the cold medium inlet is connected with one end of the combustion-supporting gas precise flow controller far away from the filter through a pipeline, the cold medium outlet is connected with the combustion-supporting gas inlet II through a pipeline, the heat medium inlet is connected with the gas outlet through a pipeline, the heat exchange sheet is used for preheating the combustion-supporting gas injected into the heat exchanger, the cold medium inlet is used for allowing the combustion-supporting gas after pressurization and filtration treatment to enter, the cold medium outlet is used for allowing the combustion-supporting gas after preheating treatment to be discharged, the heat medium inlet is used for allowing tail gas generated by the detector body to enter, and the tail gas enters the hot end of the heat exchanger through the heat medium inlet, the combustion-supporting gas entering the heat exchanger is preheated, and the heat medium outlet is used for allowing the tail gas in a low-temperature state after heat exchange to be discharged.
Further, the electrolytic reactor inner chamber is provided with the electrolysis trough, open the electrolytic reactor outside has water inlet, hydrogen export and moisturizing mouth, the water inlet passes through the pipeline and is connected with the condensate water collector, the hydrogen export is connected with the one end that the detector body was kept away from to hydrogen precision flow controller through the pipeline, the electrolysis trough is used for electrolyzing the condensate water and the water source of pouring into electrolytic reactor inside, produces hydrogen, the water inlet is used for allowing the condensate water that carries through the condensate water collector to get into, the hydrogen export is used for cooperating the pipeline and carries the hydrogen that produces to the hydrogen precision flow controller in with the electrolysis process, the moisturizing mouth is used for pouring into the water source when the system starts or pouring into the water source when the condensate water of carrying to the electrolytic reactor is not enough.
Furthermore, the combustion-supporting air pump is a diaphragm pump, the hydrogen precise flow controller and the combustion-supporting air precise flow controller are both electronic pressure controllers, the heat exchanger is a stainless steel plate type heat exchanger, the combustion-supporting air pump adopts a diaphragm pump to reduce the occupied space during the operation of the system, and completely isolating the injected combustion-supporting gas from the outside, wherein the hydrogen precise flow controller and the combustion-supporting gas precise flow controller both adopt electronic pressure controllers, can realize automatic, quantitative control to combustion-supporting gas and hydrogen, improve the control accuracy, accurate flow controller of hydrogen and the accurate flow controller of combustion-supporting gas can also adopt air-vent valve or electron flow controller, and the heat exchanger adopts stainless steel material board formula heat transfer, avoids the comdenstion water that the heat exchanger produced at the heat transfer in-process to lead to the fact the corruption to the heat exchanger inside, and then has reduced the life of heat exchanger.
Further, the filter is equipped with the molecular sieve in proper order along the gas circuit direction, allochroic silica gel and powder filter, the molecular sieve is an aluminosilicate compound that has cubic lattice, a moisture for in the combustion-supporting gas adsorbs, allochroic silica gel is used for adsorbing the vapor in the combustion-supporting gas, and whether the molecular sieve absorbs water saturation with self according to the colour change judgement molecular sieve of self, powder filter is arranged in filtering the granule in combustion-supporting gas and molecular sieve and the allochroic silica gel through the fiber filter material, prevent that fixed granule from getting into the system and blockking up the pipeline, be equipped with the molecular sieve in proper order along the gas circuit direction, allochroic silica gel and powder filter main aim at lie in: firstly, a large amount of moisture in the combustion-supporting gas is filtered through a molecular sieve, the allochroic silica gel is used as an indicator, after the allochroic silica gel changes color, the molecular sieve and the allochroic silica gel are proved to be saturated by water absorption, the molecular sieve and the allochroic silica gel need to be regenerated, and the allochroic silica gel is placed in a final powder filter and used for filtering solid particles in the combustion-supporting gas and powder generated by the molecular sieve and the allochroic silica gel.
Further, the specific detection method of the detection system of the hydrogen flame ionization detector comprises the following steps:
the method comprises the following steps: injecting combustion-supporting gas into a combustion-supporting air pump through a pipeline for pressurization, allowing the pressurized combustion-supporting gas to enter a filter through the pipeline for dewatering, filtering and purifying, allowing the purified combustion-supporting gas to enter a heat exchanger for preheating at a flow rate of 350mL/min by using a combustion-supporting gas precision flow controller, allowing the combustion-supporting gas to enter a catalytic oxidation reactor through a combustion-supporting gas inlet II for purifying again when the combustion-supporting gas is preheated to 220 ℃, allowing the purified preheated combustion-supporting gas to enter a detector body through a combustion-supporting gas outlet, the pipeline and the combustion-supporting gas inlet I, preheating the combustion-supporting gas to 220 ℃ through the heat exchanger, ensuring that the combustion-supporting gas reaches the reaction temperature of a catalytic oxidant when passing through the catalytic oxidation reactor, and reducing the heating time of the combustion-supporting gas by the detector body;
step two: injecting a water source into an electrolysis reactor through a water replenishing port through a pipeline, wherein the electrolysis reactor generates hydrogen by electrolyzing the injected water source, a hydrogen precise flow controller controls the generated hydrogen to enter a detector body through a hydrogen inlet at the flow rate of 35mL/min, and controls combustion-supporting gas and the hydrogen to be injected according to a certain proportion, so that the hydrogen flame ionization detector has high response, and the water source injected from the water replenishing port is used for ensuring that the hydrogen generated by electrolysis is enough to react with the combustion-supporting gas before condensed water is conveyed to the electrolysis reactor and is used for the condition that the condensed water in an electrolysis water tank is insufficient due to tail gas dissipation;
step three: separating sample gas to be detected by a chromatographic column, injecting the sample gas into a detector body through a chromatographic column interface, heating the detector body to 250 ℃ through a heating rod arranged in a heating rod mounting hole, enabling hydrogen and combustion-supporting gas entering the detector body to be fully combusted under a high-temperature condition, ejecting flame generated in the combustion process through a nozzle, and heating the detector body to 250 ℃ to ensure that the detector body can normally work;
step four: the temperature of tail gas generated in the combustion process of hydrogen and combustion-supporting gas is 250 ℃, the tail gas is controlled to be injected into the hot end of the heat exchanger through the gas outlet, the pipeline and the heat medium inlet at the flow rate of 400mL/min, the combustion-supporting gas is preheated, the tail gas cooled to 30 ℃ after heat exchange treatment is discharged to the atmosphere through the heat medium outlet, the tail gas is controlled to be injected into the heat exchanger at the flow rate of 400mL/min, the flow rate of the tail gas is greater than the flow rate of the combustion-supporting gas, the heat exchange between the tail gas and the combustion-supporting gas is ensured to be sufficient, the tail gas in a low-temperature state can be smoothly discharged from the heat medium outlet, the temperature of the heat medium outlet is set to be 30 ℃, the tail gas is discharged before being lower than the temperature of the combustion-supporting gas, and the adverse effect caused by the reduction of the temperature of the combustion-supporting gas at normal temperature is avoided;
step five: and repeating the first step, the third step and the fourth step to realize the circulating operation of the system, wherein about 60 percent of water can be recovered in the circulating operation process of the system, and the water replenishing period of the electrolytic reactor can be doubled.
Further, in the first step and the fourth step, the heat exchanger preheats the combustion-supporting gas, and the tail gas generates condensed water in the heat exchange process and is collected in a condensed water collector, the condensed water collector discharges the condensed water to an electrolysis reactor through a pipeline, the electrolysis reactor generates hydrogen through electrolyzing the condensed water, the hydrogen generated by the hydrogen precise flow controller is controlled to enter the detector body through a hydrogen inlet at the flow rate of 35mL/min, and when the condensed water generated in the heat exchange process is insufficient, a proper amount of water source can be supplemented through a water supplementing port to ensure the circulating operation of the system.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the environmental air which is primarily filtered by the filter and secondarily purified by the catalytic oxidation reactor is used as the combustion-supporting gas, and the detector body and the catalytic oxidation purification function are integrated into a whole, so that the integration level of the system is improved, and the volume of the system is reduced.
2. The heat generated by heating the detector body by the heating rod and the heat generated by burning the hydrogen flame are used for catalytic oxidation treatment of the combustion-supporting gas, so that the energy consumption of the system is reduced, the heat of the tail gas of the detector body and the latent heat of liquefaction of water vapor in the tail gas are recovered by heat exchange, the energy consumption of the system is reduced, and the device is green and environment-friendly.
3. According to the invention, the water generated by burning the detector body recovered by the heat exchanger and the water generated by preheating the combustion-supporting gas by the heat exchanger are used as raw materials for hydrogen production by electrolysis, so that the times of artificial water supplement can be reduced, the maintenance frequency is reduced, the circulating operation of the system can be realized to the greatest extent, the hydrogen generated in the water electrolysis process is used for providing fuel gas for the detector body, and the system integration level is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of the operating principle of the entire hydrogen flame ionization detector system with ultra-low energy and material consumption according to the present invention;
FIG. 2 is a schematic diagram of a partial system operating principle of an ultra-low energy and material consumption hydrogen flame ionization detector system of the present invention;
FIG. 3 is a schematic diagram of the base structure of an ultra low energy and material consumption hydrogen flame ionization detector system of the present invention;
FIG. 4 is a schematic cross-sectional view of a catalytic oxidation reactor of an ultra low energy and material consumption hydrogen flame ionization detector system of the present invention;
FIG. 5 is a schematic cross-sectional view of a heat exchanger of an ultra low energy and material consumption hydrogen flame ionization detector system of the present invention;
FIG. 6 is a schematic cross-sectional view of an electrolytic reactor of an ultra low energy and material consumption hydrogen flame ionization detector system of the present invention.
In the figure: 1. a detector body; 11. a base; 111. a chromatography column interface; 112. a hydrogen gas inlet; 113. a first combustion-supporting gas inlet; 114. an air outlet; 115. a heating rod mounting hole; 116. a temperature sensor mounting hole; 12. a nozzle; 13. a collector; 14. a catalytic oxidation reactor; 141. a catalytic oxidizing agent; 142. a combustion-supporting gas inlet II; 143. a combustion-supporting gas outlet; 15. a heat-insulating layer; 2. a heat exchanger; 21. a heat exchanger fin; 22. a cold medium inlet; 23. a cold medium outlet; 24. a thermal medium inlet; 25. a thermal medium outlet; 3. a condensed water collector; 4. an electrolysis reactor; 41. an electrolytic cell; 42. a water inlet; 43. a hydrogen outlet; 44. a water replenishing port; 5. a hydrogen gas precision flow controller; 6. a precise flow controller of combustion-supporting gas; 7. a filter; 8. a combustion-supporting air pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-6, the present invention provides the following technical solutions: comprises a detector body 1, the detector body 1 comprises a base 11, a nozzle 12, a collector 13, a catalytic oxidation reactor 14 and a heat preservation layer 15, the detector body 1 is used for matching a heat exchanger 2 and an electrolytic reactor 4 to detect sample gas to be detected, and heat generated in the processes of self-heating and hydrogen flame combustion is transmitted to the catalytic oxidation reactor 14, the catalytic oxidation reactor 14 is ensured to carry out effective catalytic oxidation treatment on combustion-supporting gas, the base 11 is used for installing the nozzle 12 and the collector 13, the nozzle 12 and the collector 13 are arranged on the base 11, the collector 13 is positioned above flame generated by the nozzle 12, the nozzle 12 is used for spraying flame generated in the combustion process of hydrogen and combustion-supporting gas, and allowing the hydrogen and the sample gas to enter the detector body 1 from the bottom after being communicated internally, the combustion-supporting gas is allowed to enter the detector body 1 from the middle upper part, the collector 13 is used for receiving ionization signals generated in the flame sprayed by the nozzle 12, and the collector 13 is insulated from the base 11, avoid the existence of an electric field between the collector and the base, and influence the detection result, the catalytic oxidation reactor 14 and the base 11 are integrally formed, and the catalytic oxidation reactor 14 is positioned at the outer side of the collector 13, the catalytic oxidation reactor 14 purifies the preheated combustion-supporting gas through the catalytic oxidant 141 filled inside, and the indexes such as noise, detection limit and the like of the detector body 1 are obviously influenced by the too low cleanliness of the combustion-supporting gas, so that the detection effect of the detector body 1 is reduced, the outer side of the base 11 and the catalytic oxidation reactor 14 are sleeved with the heat-insulating layer 15, and the heat-insulating layer 15 is used for reducing the heat loss generated in the detector body 1.
The bottom of the base 11 is provided with a chromatographic column interface 111, the chromatographic column interface 111 is used for enabling a sample gas to be detected after being separated by a chromatographic column to enter, one side of the base 11 is provided with a hydrogen gas inlet 112 and a combustion-supporting gas inlet 113, the combustion-supporting gas inlet 113 is positioned above the hydrogen gas inlet 112, the hydrogen gas inlet 112 is used for enabling hydrogen generated after water electrolysis of the electrolysis reactor 4 to enter, the combustion-supporting gas inlet 113 is used for enabling combustion-supporting gas purified by the catalytic oxidation reactor 14 to enter, the top of the base 11 is provided with a gas outlet 114, the gas outlet 114 is used for transmitting tail gas generated by combustion in the detector body 1 to the heat exchanger 2 through a pipeline, one side of the base 11 is provided with a heating rod mounting hole 115 and a temperature sensor mounting hole 116, the temperature sensor mounting hole 116 is positioned around the heating rod mounting hole 115, the heating rod mounting hole 115 is used for mounting a heating rod, the mounted heating rod is heated to 250 ℃, the hydrogen and the combustion-supporting gas injected into the detector body 1 are combusted, the temperature sensor mounting hole 116 is used for mounting a temperature sensor, the temperature inside the detector body 1 is measured, and insufficient combustion of the hydrogen and the combustion-supporting gas is avoided.
The catalytic oxidation reactor 14 inner chamber is filled with catalytic oxidation agent 141, catalytic oxidation agent 141 is used for purifying the combustion-supporting gas of pouring into the catalytic oxidation reactor 14 inside, catalytic oxidation reactor 14 outside is opened has combustion-supporting gas import two 142 and combustion-supporting gas export 143, combustion-supporting gas export 143 is used for being connected with combustion-supporting gas import one 113 through the pipeline, will carry the combustion-supporting gas after catalytic oxidation agent 141 purifies to detector body 1, combustion-supporting gas import two 142 is connected with the cold medium export 23 that sets up on the heat exchanger 2 through the pipeline, combustion-supporting gas import two 142 is used for making the combustion-supporting gas after the heat exchanger 2 preheats get into.
The hydrogen flame ionization detector system also comprises a heat exchanger 2, a condensate water collector 3, an electrolytic reactor 4, a hydrogen gas precise flow controller 5, a combustion-supporting gas precise flow controller 6, a filter 7 and a combustion-supporting air pump 8, wherein the heat exchanger 2 is respectively connected with the detector body 1 and the combustion-supporting gas precise flow controller 6 through pipelines, the heat exchanger 2 is used for preheating injected combustion-supporting gas, exhausting low-temperature tail gas to the atmosphere and conveying condensate water generated in the heat exchange process to the condensate water collector 3, the condensate water collector 3 is installed on the heat exchanger 2, the condensate water collector 3 is connected with the electrolytic reactor 4 through a pipeline, the condensate water collector 3 is used for collecting the condensate water and exhausting the collected condensate water to the electrolytic reactor 4, the electrolytic reactor 4 is connected with one end of the hydrogen gas precise flow controller 5, which is far away from the detector body 1, through a pipeline, the electrolytic reactor 4 is used for electrolyzing water source injected from the water replenishing port 44 or condensed water conveyed from the condensed water collector 3, and conveying hydrogen generated after electrolysis to the hydrogen precise flow controller 5, one end of the hydrogen precise flow controller 5 far away from the electrolytic reactor 4 is connected with the detector body 1 through a pipeline, the hydrogen precise flow controller 5 is used for adjusting the hydrogen amount injected into the detector body 1, one end of the combustion-supporting gas precise flow controller 6 is connected with the heat exchanger 2 through a pipeline, the combustion-supporting gas precise flow controller 6 is used for adjusting the combustion-supporting gas amount injected into the heat exchanger 2, the other end of the combustion-supporting gas precise flow controller 6 is connected with the filter 7 through a pipeline, the filter 7 is used for filtering water and fixed particles in the combustion-supporting gas, one end of the filter 7 far away from the combustion-supporting gas precise flow controller 6 is connected with the combustion-supporting gas pump 8 through a pipeline, the combustion-supporting air pump 8 is used for pressurizing combustion-supporting air injected from the outside, and ensures that the injected combustion-supporting air is enough to react with hydrogen.
A heat exchange sheet 21 is installed inside the heat exchanger 2, the heat exchange sheet 21 is used for preheating combustion-supporting gas injected into the heat exchanger 2, a cold medium inlet 22, a cold medium outlet 23, a heat medium inlet 24 and a heat medium outlet 25 are formed in the outer side of the heat exchanger 2, the cold medium inlet 22 is connected with one end, far away from the filter 7, of the combustion-supporting gas precision flow controller 6 through a pipeline, the cold medium inlet 22 is used for allowing the combustion-supporting gas subjected to pressurization and filtration treatment to enter, the cold medium outlet 23 is connected with the combustion-supporting gas inlet II 142 through a pipeline, the cold medium outlet 23 is used for allowing the combustion-supporting gas subjected to preheating treatment to be discharged, the heat medium inlet 24 is connected with the gas outlet 114 through a pipeline, the heat medium inlet 24 is used for allowing tail gas generated by the detector body 1 to enter, the tail gas enters the hot end of the heat exchanger 2 through the heat medium inlet 24 to preheat the combustion-supporting gas entering the heat exchanger 2, the heat medium outlet 25 is used for allowing the tail gas in a low temperature state after heat exchange to be discharged.
The inner cavity of the electrolytic reactor 4 is provided with an electrolytic bath 41, the electrolytic bath 41 is used for electrolyzing condensed water and water source injected into the inner part of the electrolytic reactor 4 to generate hydrogen, a water inlet 42 is arranged at the outer side of the electrolytic reactor 4, a hydrogen outlet 43 and a water replenishing port 44 are arranged, the water inlet 42 is connected with the condensed water collector 3 through a pipeline, the water inlet 42 is used for allowing condensed water conveyed by the condensed water collector 3 to enter, the hydrogen outlet 43 is connected with one end of the hydrogen precise flow controller 5 far away from the detector body 1 through a pipeline, the hydrogen outlet 43 is used for being matched with the pipeline to convey hydrogen generated in the electrolytic process to the hydrogen precise flow controller 5, and the water replenishing port 44 is used for injecting water source when the system is started or injecting water source when the condensed water conveyed to the electrolytic reactor 4 is insufficient.
The combustion-supporting air pump 8 is a diaphragm pump, the size of the space occupied by the system during operation is reduced by adopting the diaphragm pump as the combustion-supporting air pump 8, and completely isolating the injected combustion-supporting gas from the outside, wherein the hydrogen precise flow controller 5 and the combustion-supporting gas precise flow controller 6 are both electronic pressure controllers, can realize the automation to combustion-supporting gas and hydrogen, quantitative control, the control accuracy has been improved, hydrogen precision flow controller 5 and combustion-supporting gas precision flow controller 6 can also adopt air-vent valve or electron flow controller, heat exchanger 2 is stainless steel plate type heat exchanger, heat exchanger 2 adopts stainless steel plate type heat transfer, the comdenstion water of avoiding heat exchanger 2 to produce at the heat transfer in-process causes the corruption to heat exchanger 2 is inside, and then has reduced heat exchanger 2's life.
Filter 7 is equipped with the molecular sieve in proper order along the gas circuit direction, allochroic silica gel and powder filter, the molecular sieve is an aluminosilicate compound that has cubic lattice, a moisture for in the combustion-supporting gas adsorbs, allochroic silica gel is arranged in adsorbing the vapor in the combustion-supporting gas, and whether the molecular sieve absorbs water saturation with self according to the colour change judgement molecular sieve of self, powder filter is arranged in filtering the granule of combustion-supporting gas and molecular sieve and allochroic silica gel through the fiber filter material, prevent that fixed granule from getting into the system and blockking up the pipeline, be equipped with the molecular sieve in proper order along the gas circuit direction, allochroic silica gel and powder filter main aim at lie in: firstly, a large amount of moisture in the combustion-supporting gas is filtered through a molecular sieve, the allochroic silica gel is used as an indicator, after the allochroic silica gel changes color, the molecular sieve and the allochroic silica gel are proved to be saturated by water absorption, the molecular sieve and the allochroic silica gel need to be regenerated, and the allochroic silica gel is placed in a final powder filter and used for filtering solid particles in the combustion-supporting gas and powder generated by the molecular sieve and the allochroic silica gel.
Example (b): the specific detection method of the detection system of the hydrogen flame ionization detector comprises the following steps:
the method comprises the following steps: injecting combustion-supporting gas into a combustion-supporting air pump 8 through a pipeline for pressurization continuously, allowing the pressurized combustion-supporting gas to enter a filter 7 through the pipeline for water removal and filtration purification, controlling the purified combustion-supporting gas to enter a heat exchanger 2 at a flow rate of 350mL/min by a combustion-supporting gas precise flow controller 6 for preheating, allowing the combustion-supporting gas to enter a catalytic oxidation reactor 14 through a combustion-supporting gas inlet II 142 for purification again when the combustion-supporting gas is preheated to 220 ℃, allowing the purified preheated combustion-supporting gas to enter a detector body 1 through a combustion-supporting gas outlet 143, the pipeline and the combustion-supporting gas inlet I113, preheating the combustion-supporting gas to 220 ℃ through the heat exchanger 2, ensuring that the combustion-supporting gas reaches the reaction temperature of a catalytic oxidant 141 when passing through the catalytic oxidation reactor 14, and reducing the heating time of the detector body 1 on the combustion-supporting gas;
step two: injecting a water source into the electrolytic reactor 4 through a water replenishing port 44 through a pipeline, wherein the electrolytic reactor 4 generates hydrogen through electrolyzing the injected water source, the hydrogen precision flow controller 5 controls the generated hydrogen to enter the detector body 1 through a hydrogen inlet 112 at a flow rate of 35mL/min, and controls combustion-supporting gas and hydrogen to be injected according to a certain proportion, so that the hydrogen flame ionization detector has high response, the water source injected from the water replenishing port is used for ensuring that the hydrogen generated by electrolysis is enough to react with the combustion-supporting gas before condensed water is conveyed to the electrolytic reactor, and is used for the condition that the condensed water in an electrolytic water tank is insufficient due to tail gas dissipation;
step three: separating sample gas to be detected by a chromatographic column, injecting the sample gas into the detector body 1 through a chromatographic column interface 111, heating the detector body 1 to 250 ℃ through a heating rod arranged in a heating rod mounting hole 115, enabling hydrogen and combustion-supporting gas entering the detector body 1 to be fully combusted under the high-temperature condition, ejecting flame generated in the combustion process through a nozzle 12, and heating the detector body 1 to 250 ℃ to ensure that the detector body 1 can normally work;
step four: the temperature of tail gas generated in the combustion process of hydrogen and combustion-supporting gas is 250 ℃, the tail gas is controlled to be injected into the hot end of the heat exchanger 2 through the gas outlet 114, the pipeline and the heat medium inlet 24 at the flow rate of 400mL/min, the combustion-supporting gas is preheated, the tail gas cooled to 30 ℃ after heat exchange treatment is exhausted to the atmosphere through the heat medium outlet 25, the tail gas is controlled to be injected into the heat exchanger 2 at the flow rate of 400mL/min, the flow rate of the tail gas is greater than the flow rate of the combustion-supporting gas, the heat exchange between the tail gas and the combustion-supporting gas is ensured to be sufficient, the tail gas in a low-temperature state can be smoothly exhausted from the heat medium outlet 25, the temperature of the heat medium outlet is set to be 30 ℃, the tail gas is ensured to be exhausted before the temperature of the combustion-supporting gas is lower than the temperature, and the adverse effect caused by the reduction of the temperature of the combustion-supporting gas at normal temperature is avoided;
step five: and repeating the first step, the third step and the fourth step to realize the circulating operation of the system, wherein about 60 percent of water can be recovered in the circulating operation process of the system, and the water replenishing period of the electrolytic reactor 4 can be doubled.
In the first step and the fourth step, the heat exchanger 2 preheats the combustion-supporting gas, condensed water generated in the tail gas in the heat exchange process is collected in the condensed water collector 3, the condensed water is discharged to the electrolytic reactor 4 through the pipeline by the condensed water collector 3, the electrolytic reactor 4 generates hydrogen through electrolyzing the condensed water, the hydrogen precision flow controller 5 controls the generated hydrogen to enter the detector body 1 through the hydrogen inlet 112 at the flow rate of 35mL/min, and when the condensed water generated in the heat exchange process is insufficient, a proper amount of water source can be supplemented through the water supplementing port 44 to ensure the circulating operation of the system.
The working principle of the invention is as follows: when the system is started, a worker firstly starts the system, the detector body 1 is heated through the heating rod, then combustion-supporting gas is injected into the combustion-supporting gas pump 8 through a pipeline, the combustion-supporting gas pump 8 pressurizes the injected combustion-supporting gas, the pressurized combustion-supporting gas is conveyed to the filter 7 through the pipeline to carry out water removal and fixed particle filtration treatment on the combustion-supporting gas, the purified combustion-supporting gas is quantitatively conveyed to the heat exchanger 2 after being adjusted by the combustion-supporting gas precise flow controller 6, the heat exchanger 2 preheats the combustion-supporting gas, condensed water generated in the preheating process is conveyed to the electrolytic reactor 4 through the condensed water collector 3, the preheated combustion-supporting gas enters the detector body 1 from the middle upper part of the nozzle 12 after being subjected to catalytic oxidation treatment by the catalytic oxidation reactor 14, when the system is started, a water source is injected through the water replenishing port 44, and the injected water source generates hydrogen under the electrolytic action of the electrolytic reactor 4, the produced hydrogen is regulated by a hydrogen precise flow controller 5 and then quantitatively output, the hydrogen and combustion-supporting gas injected into the detector body 1 are combusted under the high-temperature condition after being communicated with the sample gas separated by a chromatographic column in the gas inlet, the flame generated in the combustion process is sprayed out from a nozzle 12, a collector 13 receives an ionization signal generated in the flame, the ionization of the hydrogen flame is further detected, tail gas generated in the combustion process is conveyed into a heat exchanger 2 through a pipeline to preheat the combustion-supporting gas, the tail gas subjected to heat exchange treatment and temperature reduction is discharged to the atmosphere from a heat medium outlet 25, a condensate water collector 3 preheats the combustion-supporting gas, the tail gas generates condensate water in the heat exchange process and is collected, the collected condensate water is conveyed to an electrolytic reactor 4 through a pipeline, the electrolytic reactor 4 generates the hydrogen by electrolyzing the condensate water, the generated hydrogen is quantitatively conveyed into the detector body 1 after being adjusted by the hydrogen precise flow controller 5, the circulating operation of the system is realized, various sample gases can be continuously detected, and the system is closed after the detection is finished.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A hydrogen flame ionization detector system with ultra-low energy and material consumption, characterized by: including detector body (1), detector body (1) includes base (11), nozzle (12), collector (13), catalytic oxidation reactor (14) and heat preservation (15), be provided with nozzle (12) and collector (13) on base (11), just collector (13) are located the flame top that nozzle (12) produced, catalytic oxidation reactor (14) and base (11) integrated into one piece, just catalytic oxidation reactor (14) are located the collector (13) outside, base (11) and catalytic oxidation reactor (14) outside cover have heat preservation (15).
2. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 1, wherein: the gas chromatography device is characterized in that a chromatographic column interface (111) is arranged at the bottom of the base (11), a hydrogen gas inlet (112) and a combustion-supporting gas inlet (113) are arranged on one side of the base (11), the combustion-supporting gas inlet (113) is positioned above the hydrogen gas inlet (112), a gas outlet (114) is arranged at the top of the base (11), a heating rod mounting hole (115) and a temperature sensor mounting hole (116) are arranged on one side of the base (11), and the temperature sensor mounting hole (116) is positioned around the heating rod mounting hole (115).
3. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 2, wherein: the catalytic oxidation reactor is characterized in that a catalytic oxidant (141) is filled in the inner cavity of the catalytic oxidation reactor (14), a combustion-supporting gas inlet II (142) and a combustion-supporting gas outlet (143) are formed in the outer side of the catalytic oxidation reactor (14), and the combustion-supporting gas outlet (143) is connected with the combustion-supporting gas inlet I (113) through a pipeline.
4. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 3, wherein: the hydrogen flame ionization detector system also comprises a heat exchanger (2), a condensate water collector (3), an electrolysis reactor (4), a hydrogen gas precise flow controller (5), a combustion-supporting gas precise flow controller (6), a filter (7) and a combustion-supporting gas pump (8), wherein the heat exchanger (2) is respectively connected with the detector body (1) and the combustion-supporting gas precise flow controller (6) through pipelines, the condensate water collector (3) is installed on the heat exchanger (2), the condensate water collector (3) is connected with the electrolysis reactor (4) through a pipeline, the electrolysis reactor (4) is connected with one end, away from the detector body (1), of the hydrogen gas precise flow controller (5), one end, away from the electrolysis reactor (4), of the hydrogen gas precise flow controller (5) is connected with the detector body (1) through a pipeline, one end of the combustion-supporting gas precise flow controller (6) is connected with the heat exchanger (2) through a pipeline, the other end of the combustion-supporting gas precise flow controller (6) is connected with the filter (7) through a pipeline, and one end, far away from the combustion-supporting gas precise flow controller (6), of the filter (7) is connected with the combustion-supporting air pump (8) through a pipeline.
5. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 4, wherein: heat exchanger (2) internally mounted has heat exchanger fin (21), open heat exchanger (2) outside has cold medium import (22), cold medium export (23), hot medium import (24) and hot medium export (25), cold medium import (22) is connected with the one end that filter (7) were kept away from in combustion-supporting gas precision flow controller (6) through the pipeline, cold medium export (23) are connected with combustion-supporting gas import two (142) through the pipeline, hot medium import (24) are connected with gas outlet (114) through the pipeline.
6. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 5, wherein: an electrolytic bath (41) is arranged in the inner cavity of the electrolytic reactor (4), a water inlet (42), a hydrogen outlet (43) and a water replenishing port (44) are formed in the outer side of the electrolytic reactor (4), the water inlet (42) is connected with the condensed water collector (3) through a pipeline, and the hydrogen outlet (43) is connected with one end, far away from the detector body (1), of the hydrogen precise flow controller (5) through a pipeline.
7. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 6, wherein: the combustion-supporting air pump (8) is a diaphragm pump, the hydrogen precise flow controller (5) and the combustion-supporting air precise flow controller (6) are both electronic pressure controllers, and the heat exchanger (2) is a stainless steel plate type heat exchanger.
8. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 7, wherein: and the filter (7) is sequentially provided with a molecular sieve, allochroic silica gel and a powder filter along the gas path direction.
9. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 8, wherein: the specific detection method of the detection system of the hydrogen flame ionization detector comprises the following steps:
the method comprises the following steps: the method comprises the steps that combustion-supporting gas is continuously injected into a combustion-supporting air pump (8) through a pipeline to be pressurized, the pressurized combustion-supporting gas enters a filter (7) through the pipeline to be subjected to water removal and filtration purification, the purified combustion-supporting gas enters a heat exchanger (2) to be preheated after the flow of the purified combustion-supporting gas is regulated through a combustion-supporting gas precise flow controller (6), the preheated combustion-supporting gas enters a catalytic oxidation reactor (14) through a combustion-supporting gas inlet II (142) to be purified again, and the purified preheated combustion-supporting gas enters a detector body (1) through a combustion-supporting gas outlet (143), the pipeline and a combustion-supporting gas inlet I (113);
step two: a water source is injected into the electrolytic reactor (4) through a water replenishing port (44) through a pipeline, the electrolytic reactor (4) generates hydrogen through electrolyzing the injected water source, and the generated hydrogen enters the detector body (1) through a hydrogen inlet (112) after the flow of the generated hydrogen is regulated by a hydrogen precise flow controller (5);
step three: separating sample gas to be detected by a chromatographic column, injecting the sample gas into the detector body (1) through a chromatographic column interface (111), heating the detector body (1) through a heating rod arranged in a heating rod mounting hole (115), burning hydrogen and combustion-supporting gas entering the detector body (1) at a high temperature, and ejecting flame generated in the burning process through a nozzle (12);
step four: tail gas generated in the combustion process of hydrogen and combustion-supporting gas is injected into the hot end of the heat exchanger (2) through the gas outlet (114), the pipeline and the heat medium inlet (24) to preheat the combustion-supporting gas, and the cooled tail gas after heat exchange treatment is discharged to the atmosphere through the heat medium outlet (25);
step five: and repeating the first step, the third step and the fourth step to realize the circulating operation of the system.
10. The ultra low energy and material consumption hydrogen flame ionization detector system of claim 9, wherein: in the first step and the fourth step, the heat exchanger (2) preheats the combustion-supporting gas, the tail gas generates condensed water in the heat exchange process and is collected in the condensed water collector (3), the condensed water collector (3) discharges the condensed water to the electrolytic reactor (4) through a pipeline, the electrolytic reactor (4) generates hydrogen through electrolyzing the condensed water, the generated hydrogen enters the detector body (1) through the hydrogen inlet (112) after the flow of the generated hydrogen is regulated by the hydrogen precise flow controller (5), and when the condensed water generated in the heat exchange process is insufficient, a proper amount of water source can be supplemented through the water supplementing port (44).
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