CN101907591B - Multi-atmosphere dynamic thermogravimetric-differential thermal analyzer and application thereof in sulfur transfer performance simulation and evaluation of flue gas - Google Patents
Multi-atmosphere dynamic thermogravimetric-differential thermal analyzer and application thereof in sulfur transfer performance simulation and evaluation of flue gas Download PDFInfo
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Abstract
The invention discloses a multi-atmosphere dynamic thermogravimetric-differential thermal analyzer which belongs to the field of petroleum refining industry and researches application thereof in sulfur transfer performance simulation and evaluation of flue gas. The analyzer comprises a protection gas circuit, a multigroup reaction gas circuit, a purging gas circuit, a switching valve, a test reactor, a drain port, a tail gas absorption device and an electrothermal furnace. The analyzer can blend and provide different required multicomponent mixed gas through one or a plurality of groups of gas regulating and mixing systems, switch the atmospheres in the test reactor according to requirements, simulate reaction atmospheres with complicated changes, realize dynamic in-situ testing, more particularly simulate a sulfur dioxide atmosphere and a hydrogen atmosphere (or a hydrocarbon atmosphere) under the micro positive pressure and carry out safe switching between the sulfur dioxide atmosphere and the hydrogen atmosphere (or the hydrocarbon atmosphere), record changes of the weight and the temperature of a sample in thermal treatment process at the real time under the condition of programmed temperature controlling, carry out thermogravimetric analysis and differential thermal analysis and is used for simulating and evaluating the performance of a sulfur transfer agent of catalytically-cracked flue gas.
Description
Technical field
The invention belongs to the petroleum refining industry field, particularly the dynamic thermogravimetric-differential thermal analyzer of one kind of multiple atmosphere can be simulated respectively multiple reaction atmosphere and betwixt flexibly switching, realizes simultaneously on-line analysis, estimates the sulphur transfer performance of catalytic cracking fuel gas sulfur transfer additive.
Background technology
Catalytic cracking process in the petrochemical industry is one of main output process of the important energy source such as gasoline, diesel oil, liquefied gas, propylene and industrial chemicals.Along with in recent years heaviness and the in poor quality of raw material, cause the inner sulfur content of raw material constantly to increase, thereby cause SOx (SO in the regeneration fume from catalytic cracking
2And SO
3General designation) discharge capacity constantly increase, cause more serious environmental pollution.Along with the increasingly stringent of legislations of environmental protection and the enhancing of environmental consciousness, must the discharging of SOx in the catalytic cracking unit be control effectively.The discharging of SOx in the regeneration fume from catalytic cracking can be obviously reduced by the use sulfur transfer additive, and the SOx in the regenerated flue gas H can be converted into
2Then S passes through Claus technique with H
2S is converted into sulphur and reclaims.Both at home and abroad the research work of sulfur transfer additive has been carried out a lot of years, the repacking thermobalances that adopt of working in advance in laboratory carry out performance evaluation and the screening of sulfur transfer additive more, and then adopt fixed bed or small-sized fluidized bed analogue means to carry out further Simulation evaluation.But because problems such as the single and standardization of burn into simulated atmosphere, never small-sized performance evaluation and screening installation moulding, convenient and flexible operation appear on the market.
Generate sulfate for the oxidation-adsorption sulphuric dioxide of sulfur transfer additive and then under hydrogen or hydrocarbon atmosphere, sulfate reduction become this process of sulfuretted hydrogen, utilize TG-DTA analysis (TG-DTA) to study this process to have simply, easily and fast, accurately, cheap characteristics.The thermogravimetric curve that obtains is processed, can be calculated sulphur load capacity and the reducing power of sulfur transfer additive, for the performance evaluation of sulfur transfer additive is screened the simple and efficient method that provides with filling a prescription.Can find the optimal oxidation-adsorption temperature of sulfur transfer additive and reduction temperature in conjunction with thermogravimetric curve and differential thermal curve.
At present, most TG-DTA analysers have the atmosphere control system, can control easy atmosphere, but gas circuit is simple, switching mode is dull, Simulation of Complex atmosphere needs the allotment by calibrating gas, very flexible and expensive, and be difficult to steady in a long-term the realization for aggressive atmosphere, flammable atmosphere.Especially for the working environment of simulation catalytic cracking fuel gas sulfur transfer additive, oxidizing sulfur dioxide atmosphere and atmosphere of hydrogen (or hydrocarbon atmosphere) are difficult to stable simulation and freely switch.The method that some solution is taked to join gas reaches the purpose of stable simulation atmosphere, if still need simulation Various Complex atmosphere just to need multiple gas, difficulty is large, and cost is high.
Summary of the invention
Purpose of the present invention solves existing atmosphere control problem in the above-mentioned TG-DTA analytical instrument exactly; provide one kind of multiple atmosphere dynamic thermogravimetric-differential thermal analyzer; this instrument possesses one or more groups gas regulation and commingled system; under the condition that protection gas is arranged, can also pass into various atmosphere---such as aggressive atmosphere, flammable atmosphere etc., can and can under multiple atmosphere, switch in one or more atmosphere atmosphere of normal pressure, pressure-fired or negative pressure Imitating.During test, under the temperature programmed control condition, can be controlled under the complicated atmosphere by atmosphere, the variation of the weight of sample and temperature in the real time record heat treatment process, and carry out thermogravimetric analysis and differential thermal analysis (DTA), reach the purpose of the dynamic in-situ test under the complicated atmosphere.Because the flexible and changeable adjustability of atmosphere, the present invention is to the simulation of Various Complex atmosphere, and is especially more true to nature to the simulation of catalytic cracking reaction regenerative process, improved the reliability of data and conclusion.The present invention can also be applied to other gas-solid reaction simulation test process that complicated atmosphere demand is arranged.
As shown in Figure 1, the dynamic thermogravimetric-differential thermal analyzer of multiple atmosphere provided by the invention comprises protection gas circuit, many group reactions gas circuit, purges gas circuit, transfer valve, test reactor, evacuation port, device for absorbing tail gas, electrothermal furnace.Crucible and the reference crucible of placing sample are arranged in the test reactor, and crucible is placed on the support bar.Blanket gas connects pressure maintaining valve, flow stabilizing valve, flowmeter, balance container successively in the protection gas circuit, then protects the lower end of gas circuit connecting test reactor; Purge purge gas connection pressure maintaining valve, flow stabilizing valve, flowmeter, mixer in the gas circuit, then purge gas circuit and connect transfer valve; Every kind of reacting gas of the every group reaction gas circuit in many group reactions gas circuit connects pressure maintaining valve, flow stabilizing valve, flowmeter, then connects into mixer, and mixer connects transfer valve; The upper end of transfer valve connecting test reactor; Evacuation port is positioned at the lower end of test reactor, and the back connects device for absorbing tail gas, and is then emptying.
Blanket gas and purge gas are inert gas, comprise nitrogen or argon gas.
Connect vacuum equipment after the device for absorbing tail gas of the dynamic thermogravimetric-differential thermal analyzer of above-mentioned multiple atmosphere, the gas in the vacuum-pumping exchange system or make that test reactor is inner to keep certain negative pressure.
Can increase one or more in gas concentration on-line detector device, gas chromatography, the mass spectrum between the evacuation port of the dynamic thermogravimetric-differential thermal analyzer of above-mentioned multiple atmosphere and the device for absorbing tail gas, form instant or the accumulative total analysis to the tail gas of discharging, in conjunction with TG-DTA data analysis reaction process.
Blanket gas and reacting gas are divided into two-way and independently enter test reactor; blanket gas directly enters the balance container; discharge from evacuation port with the reacting gas that is come by test reactor again; can avoid reacting gas to enter the balance container on the one hand; cause corrosion or pollution to the accurate device of balance inside; can avoid on the other hand blanket gas to enter the reaction zone of test reactor, prevent from the composition of reaction gas is produced interference, destroy the stable of reaction atmosphere.In test process, can carry out as required the switching of different atmosphere, if the reaction that may occur not expect between two kinds of to be switched atmosphere then can be carried out first inert gas purge between switching.
Dynamic thermogravimetric-the differential thermal analyzer of multiple atmosphere provided by the invention is in the application of Simulation evaluation flue gas sulphur transfer performance.Specifically can simulate sulphuric dioxide atmosphere (oxidation-adsorption sulphuric dioxide generates sulfate) and hydrogen or hydrocarbon atmosphere (sulfate reduction is become sulfuretted hydrogen), estimate the sulphur transfer performance of catalytic cracking fuel gas sulfur transfer additive.Utilize the method for the dynamic thermogravimetric of multiple atmosphere of the present invention-differential thermal analyzer Simulation evaluation flue gas sulphur transfer performance: as shown in Figure 2, the crucible that fills the sulfur transfer additive sample is placed on the sample support bar, and put the reference crucible well, assemble after test reactor and all gas circuits, pass into blanket gas through pressure maintaining valve, flow stabilizing valve, flowmeter to the balance container, then enter test reactor from the lower end; Then purge gas passes into test reactor from the upper end, the exchange system air through pressure maintaining valve, flow stabilizing valve, flowmeter, mixer; Every kind of reacting gas mixes forming combination gas by pressure maintaining valve, flow stabilizing valve, flowmeter in every group reaction gas circuit in mixer, enters the measurement reactor from the upper end, forms the required atmosphere atmosphere of experiment; Transfer valve can and purge between the gas circuit in different group reaction gas circuits and switch; The electrothermal furnace temperature programme; All gas enters behind the device for absorbing tail gas emptying by evacuation port.
Described reaction gas circuit can be oxidizing gas mixture or reduction mixed gas.Oxidizing gas mixture is nitrogen, sulphuric dioxide, oxygen mixed gas, simulation catalytic cracking regenerator atmosphere, and the oxidized absorption of simulation sulphuric dioxide forms the reaction of sulfate.The reduction mixed gas is nitrogen, hydrogen or propane mixed gas; Simulation catalytic cracking riser reactor atmosphere; Simulation sulfate is reduced into the reaction of sulfuretted hydrogen.Analyze the weight change situation of sulfur transfer additive, can assess, screen its sulphur transfer performance such as oxidation-adsorption speed, oxidation-adsorption saturated capacity, rate of reduction, reducing degree etc.
Described blanket gas and purge gas are inert gas, comprise nitrogen or argon gas.
Dynamic thermogravimetric-the differential thermal analyzer of multiple atmosphere of the present invention's design; its advantage is that required different polycomponent mixed gas be allocated and be provided to this instrument can with commingled system by one or more groups gas regulation; under the prerequisite that the inner accurate device of protection balance is not corroded; can switch as required the atmosphere in the test reactor; the reaction atmosphere that Simulation of Complex changes is realized dynamic in-situ test.For the simulation production technology, the trial-production new product, Fast Evaluation, screening provide stronger analog capability and research means.
Description of drawings
The dynamic thermogravimetric of multiple atmosphere that Fig. 1 designs for the present invention-differential thermal analyzer flow diagram.
The flow diagram of the dynamic thermogravimetric of multiple atmosphere that Fig. 2 designs for the present invention-differential thermal analyzer simulated flue gas sulfur transfer additive performance evaluation.
Embodiment
Below 2 describe in detail by reference to the accompanying drawings with embodiment.
Embodiment 1:
As shown in Figure 2, utilize the dynamic thermogravimetric of multiple atmosphere of the present invention-differential thermal analyzer simulation sulphuric dioxide oxidized absorption under the effect of sulfur transfer additive to form the process of sulfate.The crucible that fills the sulfur transfer additive sample is placed on the sample support bar, and put the reference crucible well, assemble after test reactor and all gas circuits, pass into blanket gas nitrogen through pressure maintaining valve, flow stabilizing valve, flowmeter to the balance container, then enter test reactor from the lower end; Pass into purge gas nitrogen, exchange system air through pressure maintaining valve, flow stabilizing valve, flowmeter, mixer from the test reactor upper end; After displacement is clean, the blanket gas that keeps constant rate, transfer valve will purge gas circuit and switch to the reaction gas circuit, and reacting gas nitrogen, sulphuric dioxide, oxygen form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end; The electrothermal furnace start program heats up, and carries out simultaneously dynamic in-situ test; All gas is entered behind the device for absorbing tail gas emptying by evacuation port, device for absorbing tail gas adopts sodium hydroxide lye to absorb.Simulation reaction is used the purge gas nitrogen blowing after finishing, and is cooled to simultaneously room temperature.Also drawn by computer acquisition, record, operational data in the test process, analyze weight change situation and the thermal change situation of sulfur transfer additive, can analyze the maximum oxidation adsorbance that under a certain proportion of reaction gas condition sulfur transfer additive begins temperature, the temperature variant situation of oxidation-adsorption speed and the sulphuric dioxide of oxidation-adsorption sulphuric dioxide.
Embodiment 2:
As shown in Figure 2, utilize the dynamic thermogravimetric of multiple atmosphere of the present invention-differential thermal analyzer simulation sulphuric dioxide oxidized absorption under the effect of sulfur transfer additive to form sulfate and then be reduced into the process of sulfuretted hydrogen.The crucible that fills the sulfur transfer additive sample is placed on the sample support bar, and put the reference crucible well, assemble after test reactor and all gas circuits, pass into the blanket gas argon gas through pressure maintaining valve, flow stabilizing valve, flowmeter to the balance container, then enter test reactor from the lower end; Pass into purge gas argon gas, exchange system air through pressure maintaining valve, flow stabilizing valve, flowmeter, mixer from the test reactor upper end; After displacement is clean, the blanket gas and the purge gas that keep constant rate, the electrothermal furnace temperature programme begins constant temperature after simulating the catalytic cracking regenerator temperature, transfer valve will purge gas circuit and switch to the oxidation reaction gas that reacts in the gas circuit, oxidation reaction gas nitrogen, sulphuric dioxide, oxygen form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end, the oxidized absorption of simulation sulphuric dioxide forms the reaction of sulfate; Use the purge gas argon purge after reaction reaches capacity, be cooled to simultaneously room temperature; The blanket gas that keeps constant rate, transfer valve will purge gas circuit and switch to reduction reaction gas gas circuit, reduction reaction gas nitrogen, propane form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end, electrothermal furnace again start program intensification carries out dynamic in-situ test, and maximum temperature is set to 700 ℃; All gas is entered behind the device for absorbing tail gas emptying by evacuation port, device for absorbing tail gas adopts sodium hydroxide lye and hydrogen peroxide to absorb.Simulation reaction is used the purge gas argon purge after finishing, and is cooled to simultaneously room temperature.Also drawn by computer acquisition, record, operational data in the test process, analyze weight change situation and the thermal change situation of sulfur transfer additive, can analyze the temperature variant situation of initial temperature, rate of reduction that the sulfate of formation is reduced after the sulfur transfer additive oxidation-adsorption sulphuric dioxide under a certain proportion of reaction gas condition and be reduced degree.
Embodiment 3:
As shown in Figure 2, utilize the dynamic thermogravimetric of multiple atmosphere of the present invention-differential thermal analyzer simulation sulphuric dioxide oxidized absorption under the effect of sulfur transfer additive to form sulfate and then be reduced into the process of sulfuretted hydrogen.The crucible that fills the sulfur transfer additive sample is placed on the sample support bar, and put the reference crucible well, assemble after test reactor and all gas circuits, pass into blanket gas nitrogen through pressure maintaining valve, flow stabilizing valve, flowmeter to the balance container, then enter test reactor from the lower end; Pass into purge gas argon gas, exchange system air through pressure maintaining valve, flow stabilizing valve, flowmeter, mixer from the test reactor upper end; After displacement is clean, the blanket gas and the purge gas that keep constant rate, the electrothermal furnace temperature programme begins constant temperature after simulating the catalytic cracking regenerator temperature, transfer valve will purge gas circuit and switch to the reaction gas circuit, reacting gas nitrogen, sulphuric dioxide, oxygen form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end, the oxidized absorption of simulation sulphuric dioxide forms the reaction of sulfate; Use the purge gas argon purge behind the reaction certain hour, be cooled to simultaneously simulation catalytic cracking riser reactor temperature and begin constant temperature; Transfer valve will purge gas circuit and switch to reduction reaction gas gas circuit, reduction reaction gas nitrogen, hydrogen form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end, simulation sulfate is reduced into the reaction of sulfuretted hydrogen; Switching to purge gas after the reaction certain hour purges again, be warming up to simulation catalytic cracking regenerator temperature and begin constant temperature, transfer valve will purge gas circuit and switch to the reaction gas circuit, reacting gas nitrogen, sulphuric dioxide, oxygen form mixed gas by mixing after pressure maintaining valve, flow stabilizing valve, the flowmeter respectively in mixer, enter the measurement reactor from the upper end, the oxidized absorption of simulation sulphuric dioxide forms the reaction of sulfate, and the oxidation-adsorption that so carries out next round becomes sulfate-the be reduced into circulation of sulfuretted hydrogen; All gas is entered behind the device for absorbing tail gas emptying by evacuation port, device for absorbing tail gas adopts sodium hydroxide lye to absorb.By computer acquisition, record, operational data and drawing, analyze the weight change situation of sulfur transfer additive in the test process, its sulphur transfer performance is assessed, screened.
Claims (5)
1. a method of utilizing the dynamic thermogravimetric of multiple atmosphere-differential thermal analyzer Simulation evaluation flue gas sulphur transfer performance is characterized in that,
Dynamic thermogravimetric-the differential thermal analyzer of described multiple atmosphere comprises protection gas circuit, many group reactions gas circuit, purges gas circuit, transfer valve, test reactor, evacuation port, device for absorbing tail gas, electrothermal furnace; Crucible and the reference crucible of placing sample are arranged in the test reactor, and crucible is placed on the support bar; Blanket gas connects pressure maintaining valve, flow stabilizing valve, flowmeter, balance container successively in the protection gas circuit, then protects the lower end of gas circuit connecting test reactor; Purge purge gas connection pressure maintaining valve, flow stabilizing valve, flowmeter, mixer in the gas circuit, then purge gas circuit and connect transfer valve; Every kind of reacting gas of the every group reaction gas circuit in many group reactions gas circuit connects pressure maintaining valve, flow stabilizing valve, flowmeter, then connects into mixer, and mixer connects transfer valve; The upper end of transfer valve connecting test reactor; Evacuation port is positioned at the lower end of test reactor, and the back connects device for absorbing tail gas, and is then emptying;
The method of described Simulation evaluation flue gas sulphur transfer performance is: the crucible that fills the sulfur transfer additive sample is placed on the sample support bar, and put the reference crucible well, assemble after test reactor and all gas circuits, pass into blanket gas through pressure maintaining valve, flow stabilizing valve, flowmeter to the balance container, then enter test reactor from the lower end; Then purge gas passes into test reactor from the upper end, the exchange system air through pressure maintaining valve, flow stabilizing valve, flowmeter, mixer; Every kind of reacting gas mixes forming combination gas by pressure maintaining valve, flow stabilizing valve, flowmeter in every group reaction gas circuit in mixer, enters test reactor from the upper end, forms the required atmosphere atmosphere of test; Transfer valve can and purge between the gas circuit in different group reaction gas circuits and switch; The electrothermal furnace temperature programme; All gas enters behind the device for absorbing tail gas emptying by evacuation port.
2. method according to claim 1 is characterized in that, connects vacuum equipment after the device for absorbing tail gas of the dynamic thermogravimetric-differential thermal analyzer of described multiple atmosphere.
3. any described method according to claim 1 and 2 is characterized in that, increases in gas concentration on-line detector device, gas chromatography, the mass spectrum one or more between the evacuation port of the dynamic thermogravimetric-differential thermal analyzer of described multiple atmosphere and the device for absorbing tail gas.
4. a kind of method of utilizing the dynamic thermogravimetric of multiple atmosphere-differential thermal analyzer Simulation evaluation flue gas sulphur transfer performance according to claim 1, it is characterized in that, described reaction gas circuit is oxidizing gas mixture or reduction mixed gas, oxidizing gas mixture is nitrogen, sulphuric dioxide, oxygen mixed gas, simulation catalytic cracking regenerator atmosphere, the oxidized absorption of simulation sulphuric dioxide forms the reaction of sulfate; The reduction mixed gas is nitrogen, hydrogen or propane mixed gas, simulation catalytic cracking riser reactor atmosphere, and simulation sulfate is reduced into the reaction of sulfuretted hydrogen.
5. according to claim 1 or 4 any described a kind of methods of utilizing the dynamic thermogravimetric of multiple atmosphere-differential thermal analyzer Simulation evaluation flue gas sulphur transfer performance, it is characterized in that, described blanket gas and purge gas are inert gas, comprise nitrogen or argon gas.
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| CN109490360A (en) * | 2018-12-29 | 2019-03-19 | 中国科学技术大学 | It is a kind of suitable for large sample amount, more atmosphere can be with differential thermal analysis device |
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