CN106336910A - Method for utilizing microwave in-situ synthesis to prepare zinc-ferrite desulfurizing agent - Google Patents

Method for utilizing microwave in-situ synthesis to prepare zinc-ferrite desulfurizing agent Download PDF

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CN106336910A
CN106336910A CN201610916039.7A CN201610916039A CN106336910A CN 106336910 A CN106336910 A CN 106336910A CN 201610916039 A CN201610916039 A CN 201610916039A CN 106336910 A CN106336910 A CN 106336910A
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desulfurizing agent
microwave
desulfurizing
zinc
zinc ferrite
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米杰
冯宇
李阳
武蒙蒙
鲍卫仁
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/002—Removal of contaminants
    • C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
    • C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/20—Purifying combustible gases containing carbon monoxide by treating with solids; Regenerating spent purifying masses

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a method for utilizing microwave in-situ synthesis to prepare a zinc-ferrite desulfurizing agent. A solid-phase iron and zinc synthesizing oxalic acid is mixed with a red soil carrier to prepare a desulfurizing agent precursor; in a microwave environment, the desulfurizing agent precursor is firstly roasted to perform decomposition, then constant low temperature vulcanization is performed in a simulated Texaco coal gas atmosphere, finally in-situ regeneration curing is performed in an oxygen-bearing atmosphere to obtain the fresh medium-and-high temperature coal gas desulfurizing agent. By the adoption of the zinc-ferrite desulfurizing agent, the problems of vulcanization activity reduction and desulfurizing agent internal structure powdering occurred in the vulcanization-regeneration cycling process are solved, the sulfur capacity utilization rate and mechanical strength of the desulfurizing agent are improved, the single-time sulfur capacity of the desulfurizing agent is kept above 11%, the desulfurizing efficiency is still kept above 97% after ten times of vulcanization-regeneration cycling, and the mechanical strength is above 160 N/cm.

Description

A kind of synthetic method of preparing zinc ferrite desulfurization agent of microwave in-situ of utilizing
Technical field
The invention belongs to Coal Chemical Industry desulfurizing agent preparing technical field, relate to a kind of preparation side of middle desulfurizing agent for high-temp gasMethod, particularly a kind of method of preparing zinc ferrite desulfurization agent based on microwave.
Background technology
The economic development of China, future source of energy consumption will keep the trend of rapid growth, taking coal as the main energyConsumptio is difficult to change in a short time, administer haze weather, improves efficiency of energy utilization, strengthens the clean utilization gesture of coalMust go. The clean conversion of coal resources is China's economy, social sustainable development and eco-friendly heavy with efficient technique of rainwater utilizationWant energy utilization technology, the new skills of generating such as Integrated gasification combined cycle generating (IGCC), molten carbonate fuel cell (CMFC)The coal-based Poly-generation new technology of art and artificial oil, alcohol-ether fuel combines eco-friendly Coal Gasification Technology and high efficiency combustion gasSteam combined cycle power generating technology, has realized efficient, the clean utilization of coal, be 21 century the most promising Filter Tuber For Clean Coal send outOne of power technology. But the existence of coal gasification product medium sulphide content not only can be corroded gas turbine blades, be discharged into after atmosphere,Also can serious environment pollution, harm humans health. Therefore, the research and development of middle coal gas of high temperature desulfur technology are that coal resources are cleanIndispensable important step in clean conversion system, is the key that realizes coal high-efficiency, clean utilization, prepares that Sulfur capacity is high, regenerationDesulfurizing agent quick and stable performance has important theory and practical value.
Middle coal gas of high temperature desulfurization is single metal oxide (iron oxide, zinc oxide, the oxidation by some recyclable regenerativesCalcium etc.) or composite metal oxide can with H2The principle that S or other sulfide react to each other, utilizes metal oxide to removeMost active sulfur compounds in middle coal gas of high temperature. Along with scientific and technological progress, industrial to the requirement of desulfurizing agent moreCome highlyer, single metal oxide desulfurizer cannot satisfy the demands. For high-temperature metallic oxide desulfurizing agent in improvingDesulfurization performance, the research of metal oxide desulfurizer in recent years has turned to composite metal oxide (by different metal oxidesMix or compoundly obtain a kind of new desulfurizing agent), and abundant experimental results shows, no matter is structural property or vulcanization reactionActivity, composite metal oxide all shows the advantage more incomparable than single metal oxide. Composite metal oxideAdvantage is mainly reflected in the following aspects: the Sulfur capacity that 1) increases desulfurizing agent; 2) desulfuration efficiency of raising desulfurizing agent; 3) reduce orStop the volatilization of free state metal oxide or loss; 4) can sieve and silica-sesquioxide serve as the carrier of desulfurizing agent, increase desulfurizing agentSpecific surface and hole, the decentralization of raising desulfurizer active component; 5) improve the structural stability of desulfurizing agent and strengthen desulfurizing agentMechanical strength, for desulfurizing agent large-scale industrial application is laid a solid foundation. The kind of composite metal oxide is a lot, typically compoundMetal oxide comprises: zinc ferrite, zinc titanate, iron calcium base, copper manganese base etc. And zinc ferrite and zinc titanate are the focuses of current researchAnd emphasis.
Microwave, as a kind of electromagnetic wave, is widely used in field of material preparation. Heating using microwave have heating fast and evenly,The advantages such as the features such as energy-conservation, unique microwave effect are energy-efficient, low reaction activation energy, and the suction ripple of different material mediumAbility there are differences, by regulating the structure that can effectively control synthetic material about the parameter of microwave. Heating using microwave also can addThe yield of the reaction rate of some chemical reaction, Reaction time shorten, raising product and selective soon, this is mainly owing to uniquenessMicrowave effect, comprising hot spot-effect, selective heating effect, non-thermal effect etc. In addition microwave have promote ion moveThe ability of moving, spreading. Therefore, adopt microwave can effectively reduce sulfuration as the enhancements in desulfurization and regenerative processIon diffusional resistance, raising reaction rate with regenerative process.
Dry method high temperature gas desulfurizer will adapt to the demand of commercial Application, must possess following feature: 1) high de-Sulphur precision and Sulfur capacity; 2) strong mechanical strength and stability; 3) excellent regenerability; 4) raw material being easy to get and low being prepared intoThis. The ubiquitous problem of current dry-desulphurizer is that desulfurizer active component utilization rate is lower, causes the effective of desulfurizing agentSulfur capacity is lower. In restriction, the industrialized crux of desulfurizing agent for high-temp gas is desulfurizing agent structural instability, bad mechanical strength, easyThe desulfurizing agent desulfuration efficiency that efflorescence etc. cause reduces and recycles number of times and reduces. Therefore, how to improve the sulphur of unit desulfurizing agentAppearance and desulfuration efficiency just seem particularly important. Select rational desulfurizing agent preparation condition, keep the stable of Sulfur capacity and mechanical strengthProperty, be desulfurizing agent for high-temp gas desulfurization performance and the key that recycles performance in improving.
ZL 201410176695.9 discloses a kind of method of utilizing process for solid-phase microwave synthesis to prepare zinc ferrite desulfurization agent,Desulfurizing agent single Sulfur capacity prepared by the method is about 9.75%. But, the Sulfur capacity of desulfurizing agent prepared by the method and Sulfur capacity utilization rateRelatively low, and in repeatedly vulcanizing regeneration, desulfurizing agent structural deterioration is serious, and mechanical strength significantly reduces, and is attended by certainPowder phenomenon-tion, causes desulfurizing agent sulfuration and regeneration cycle hydraulic performance decline.
Summary of the invention
The object of this invention is to provide a kind of synthetic method of preparing zinc ferrite desulfurization agent of microwave in-situ of utilizing, de-to improveSulfur capacity utilization rate and the mechanical strength of sulphur agent, the sulfuration that the agent of solution zinc ferrite desulfurization occurs in sulfuration-regeneration cycle process is livedProperty reduces and the problem of desulfurizing agent internal structure efflorescence.
The present invention utilizes microwave in-situ synthetic method to prepare zinc ferrite desulfurization agent as middle desulfurizing agent for high-temp gas, itsConcrete preparation method is:
1), the oxalate compound of the synthetic iron of solid phase and zinc, be mixed with and obtain desulfurizing agent presoma with laterite carrier;
2), at 250～350 DEG C desulfurizing agent presoma described in roasting, desulfurizing agent presoma is decomposed;
3), the desulfurizing agent presoma of described decomposition is placed under simulation Texaco coal gas atmosphere, is heated to 350～450 DEG C and carries outCryogenic thermostat sulfuration, obtains desulfurizing agent precursor;
4), described desulfurizing agent precursor carried out to in-situ regeneration under the oxygen-containing atmosphere of 550～700 DEG C solidify, obtain fresh inDesulfurizing agent for high-temp gas.
In above method, described desulfurizing agent presoma decomposes, cryogenic thermostat vulcanizes and desulfurizing agent precursor in-situ regenerationCuring process is all carried out under microwave environment.
Preferably, the microwave frequency that microwave environment of the present invention adopts is 2450MHz, microwave power 1000W.
Wherein, the consumption of described laterite carrier is 50～65% of desulfurizing agent gross mass.
The present invention is taking zinc salt, molysite and oxalic acid as raw material, the oxalate compound of the synthetic iron of solid phase and zinc, described zinc salt,Molysite is preferably 1: 1.8 with the mole dosage ratio of oxalic acid～and 2.2: 3.6～4.2.
Its concrete solid phase building-up process is, after described zinc salt, molysite and oxalic acid are mixed, to grind it is fully reacted, willProduct is 80～130 DEG C of oven dry.
Described grinding is carried out in ball mill, and the ball milling speed of ball mill is preferably 300～550r/min.
More specifically, the preferably oxalic acid of synthetic iron and zinc taking zinc acetate, ferric nitrate and oxalic acid as raw material solid phase of the present inventionCompound.
Equally, the desulfurizing agent presoma that the present invention is mixed with the described oxalate compound with iron and zinc and laterite carrierAlso dry at 80～130 DEG C.
By described desulfurizing agent presoma, in the time carrying out low-temperature microwave roasting for 250～350 DEG C, in presoma, active component reachesAfter decomposition temperature, resolve into iron oxide and zinc oxide.
In the oxygen-containing atmosphere that the present invention is preferably 2～8% at carrier of oxygen volume concentrations, described desulfurizing agent precursor is carried out to microwaveIn-situ regeneration solidifies. And then, in described in-situ regeneration solidification process, select the oxidation regeneration air speed of oxygen-containing atmosphere be 2000～ 5000h-1。
The zinc ferrite desulfurization agent of preparing using the inventive method, as a kind of composite metal oxide desulfurizing agent, combines oxidationThe advantage of the thick desulfurization of iron desulfurizing agent and Zinc oxide desulfurizer essence desulfurization, has improved desulfuration efficiency and the Sulfur capacity of desulfurizing agent.
Meanwhile, the occupy-place mechanism based on metal sulfide, in-situ synthesis has been reserved in the preparation process of desulfurizing agentThe larger inner space that metal oxide crystal is required, has enriched pore structure, has avoided in traditional preparation method because of oxygen sulphurDisplacement and molecular volume expand and the desulfurizing agent that causes is split up, efflorescence and pore structure obstruction, make gas reactant and the product canIn duct, pass in and out unimpededly, be beneficial to reactant and product mass transfer, further improved the desulfuration efficiency of unit desulfurizing agent.
Utilize heating using microwave to prepare desulfurizing agent, can promote ion diffusion, improve reaction efficiency; Heating using microwave can also subtractSintering Problem in few roasting process, improves porosity. Therefore the desulfurizing agent internal void structure of, preparing with the inventive method is richRichness, can keep higher mechanical strength, more than having reached 160N/cm.
Experiment is vulcanized in zinc ferrite desulfurization agent prepared by the present invention, and the single Sulfur capacity of desulfurizing agent remains on more than 11%,After ten sulfuration/regeneration cycle are used, desulfuration efficiency still remains on more than 97%.
Detailed description of the invention
Following embodiment is only the preferred technical solution of the present invention, and is not used in the present invention is carried out to any restriction. ForThose skilled in the art, the present invention can have various modifications and variations. Within the spirit and principles in the present invention all, institute doesAny amendment, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Embodiment 1
Take 2.19g zinc acetate (C4H6O4Zn·2H2O), 8.08g ferric nitrate (Fe (NO3)3·9H2O), with 5.04g oxalic acid (H2C2O4·2H2O) after mixing, in mortar, grind 1 hour, then put into ball mill 350r/min ball milling 2 hours; By ball milling materialAfter 90 DEG C of oven dry, add 4.82g laterite, continue ball milling 2 hours in ball mill, after the extrusion that adds water drying forming, taken offSulphur agent presoma. The desulfurizing agent presoma of preparation is put into microwave tube type oven, microwave power 1000W, microwave frequency are set2450MHz is warming up to 250 DEG C desulfurizing agent presoma is decomposed under nitrogen atmosphere. Simulation moral will be replaced as in microwave tube type ovenScholar's shungite gas atmosphere, continues to be warming up to 400 DEG C, with 1000h-1Sulfuration air speed constant temperature microwave vulcanization to tube furnace export hydrogen sulfideConcentration is identical with entrance concentration. After sulfuration completely, then oxygen and the nitrogen of carrier of oxygen volume concentrations 2% will be replaced as in microwave tube type ovenOxygen mixture, is warming up to 550 DEG C, with air speed 2000h-1Carry out micro wave regeneration and solidify 3 hours, obtain fresh zinc ferrite desulfurizationAgent.
Zinc ferrite desulfurization agent performance to above-mentioned preparation is evaluated, and concrete evaluation method is: first use simulation TexacoCoal gas gas, with the curing temperatures of 450 DEG C and 1000h-1Sulfuration air speed, on fixed bed, vulcanize test, re-use oxygenThe oxygen of gas volume concentrations 2% and nitrogen mixture body, under the regeneration temperature of 550 DEG C, with 2000h-1Air speed carry out desulfurizing agentRegeneration, the retrial of laying equal stress on is tested ten times. After ten sulfuration/regeneration cycle are used, the Sulfur capacity that detects zinc ferrite desulfurization agent is11.34%, desulfuration efficiency 98.23%, mechanical strength 135cN/cm.
Embodiment 2
Take 2.19g zinc acetate, 7.66g ferric nitrate, after mixing with 4.95g oxalic acid, in mortar, grind 1 hour, then put into ball milling400r/min ball milling 2 hours in machine; Ball milling material, after 90 DEG C of oven dry, is added to 5.12g laterite, continue ball milling 2 in ball millHour, after the extrusion that adds water drying forming, obtain desulfurizing agent presoma. The desulfurizing agent presoma of preparation is put into microwave tube type ovenIn, microwave power 1000W, microwave frequency 2450MHz are set, under nitrogen atmosphere, be warming up to 300 DEG C desulfurizing agent presoma is dividedSeparate. By being replaced as simulation Texaco coal gas atmosphere in microwave tube type oven, continue to be warming up to 450 DEG C, with 1500h-1Sulfuration air speedConstant temperature microwave vulcanization is identical with entrance concentration to tube furnace outlet concentration of hydrogen sulfide. After sulfuration completely, then by microwave tube type ovenThe oxygen and the nitrogen mixture body that are replaced as carrier of oxygen volume concentrations 4%, be warming up to 600 DEG C, with air speed 3000h-1Carry out micro wave regenerationSolidify 3.5 hours, obtain fresh zinc ferrite desulfurization agent.
Zinc ferrite desulfurization agent performance to above-mentioned preparation is evaluated, and concrete evaluation method is: first use simulation TexacoCoal gas gas, with the curing temperatures of 500 DEG C and 1500h-1Sulfuration air speed, on fixed bed, vulcanize test, re-use oxygenThe oxygen of gas volume concentrations 4% and nitrogen mixture body, under the regeneration temperature of 600 DEG C, with 2500h-1Air speed carry out desulfurizing agentRegeneration, the retrial of laying equal stress on is tested ten times. After ten sulfuration/regeneration cycle are used, the Sulfur capacity that detects zinc ferrite desulfurization agent is11.34%, desulfuration efficiency 97.37%, mechanical strength 155cN/cm.
Embodiment 3
Take 2.19g zinc acetate, 7.66g ferric nitrate, after mixing with 5.21g oxalic acid, in mortar, grind 1 hour, then put into ball milling450r/min ball milling 2 hours in machine; Ball milling material, after 90 DEG C of oven dry, is added to 6.11g laterite, continue ball milling 2 in ball millHour, after the extrusion that adds water drying forming, obtain desulfurizing agent presoma. The desulfurizing agent presoma of preparation is put into microwave tube type ovenIn, microwave power 1000W, microwave frequency 2450MHz are set, under nitrogen atmosphere, be warming up to 300 DEG C desulfurizing agent presoma is dividedSeparate. By being replaced as simulation Texaco coal gas atmosphere in microwave tube type oven, continue to be warming up to 400 DEG C, with 2000h-1Sulfuration air speedConstant temperature microwave vulcanization is identical with entrance concentration to tube furnace outlet concentration of hydrogen sulfide. After sulfuration completely, then by microwave tube type ovenThe oxygen and the nitrogen mixture body that are replaced as carrier of oxygen volume concentrations 6%, be warming up to 650 DEG C, with air speed 4000h-1Carry out micro wave regenerationSolidify 4 hours, obtain fresh zinc ferrite desulfurization agent.
Zinc ferrite desulfurization agent performance to above-mentioned preparation is evaluated, and concrete evaluation method is: first use simulation TexacoCoal gas gas, with the curing temperatures of 550 DEG C and 2000h-1Sulfuration air speed, on fixed bed, vulcanize test, re-use oxygenThe oxygen of gas volume concentrations 6% and nitrogen mixture body, under the regeneration temperature of 650 DEG C, with 3000h-1Air speed carry out desulfurizing agentRegeneration, the retrial of laying equal stress on is tested ten times. After ten sulfuration/regeneration cycle are used, the Sulfur capacity that detects zinc ferrite desulfurization agent is11.34%, desulfuration efficiency 98.75%, mechanical strength 160cN/cm.
Embodiment 4
Take 2.19g zinc acetate, 8.46g ferric nitrate, after mixing with 5.21g oxalic acid, in mortar, grind 1 hour, then put into ball milling500r/min ball milling 2 hours in machine; Ball milling material, after 90 DEG C of oven dry, is added to 5.92g laterite, continue ball milling 2 in ball millHour, after the extrusion that adds water drying forming, obtain desulfurizing agent presoma. The desulfurizing agent presoma of preparation is put into microwave tube type ovenIn, microwave power 1000W, microwave frequency 2450MHz are set, under nitrogen atmosphere, be warming up to 250 DEG C desulfurizing agent presoma is dividedSeparate. By being replaced as simulation Texaco coal gas atmosphere in microwave tube type oven, continue to be warming up to 350 DEG C, with 2500h-1Sulfuration air speedConstant temperature microwave vulcanization is identical with entrance concentration to tube furnace outlet concentration of hydrogen sulfide. After sulfuration completely, then by microwave tube type ovenThe oxygen and the nitrogen mixture body that are replaced as carrier of oxygen volume concentrations 8%, be warming up to 700 DEG C, with air speed 5000h-1Carry out micro wave regenerationSolidify 4.5 hours, obtain fresh zinc ferrite desulfurization agent.
Zinc ferrite desulfurization agent performance to above-mentioned preparation is evaluated, and concrete evaluation method is: first use simulation TexacoCoal gas gas, with the curing temperatures of 600 DEG C and 2500h-1Sulfuration air speed, on fixed bed, vulcanize test, re-use oxygenThe oxygen of gas volume concentrations 8% and nitrogen mixture body, under the regeneration temperature of 700 DEG C, with 3500h-1Air speed carry out desulfurizing agentRegeneration, the retrial of laying equal stress on is tested ten times. After ten sulfuration/regeneration cycle are used, the Sulfur capacity that detects zinc ferrite desulfurization agent is11.34%, desulfuration efficiency 97.63%, mechanical strength 165cN/cm.

Claims (7)

1. utilize the synthetic method of preparing zinc ferrite desulfurization agent of microwave in-situ, comprising:
1), the oxalate compound of the synthetic iron of solid phase and zinc, be mixed with and obtain desulfurizing agent presoma with laterite carrier;
2), at 250～350 DEG C desulfurizing agent presoma described in roasting, desulfurizing agent presoma is decomposed;
3), the desulfurizing agent presoma of described decomposition is placed under simulation Texaco coal gas atmosphere, is heated to 350～450 DEG C and carries outCryogenic thermostat sulfuration, obtains desulfurizing agent precursor;
4), described desulfurizing agent precursor carried out to in-situ regeneration under the oxygen-containing atmosphere of 550～700 DEG C solidify, obtain fresh inDesulfurizing agent for high-temp gas;
Wherein, described desulfurizing agent presoma decomposition, cryogenic thermostat sulfuration and the curing process of desulfurizing agent precursor in-situ regenerationAll under microwave environment, carry out.
2. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that described microwave environment adopts micro-Ripple frequency is 2450MHz, microwave power 1000W.
3. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that the consumption of described laterite carrier is50～65% of desulfurizing agent gross mass.
4. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that according to zinc salt, molysite and oxalic acidMole dosage ratio is 1: 1.8～2.2: 3.6～4.2, the oxalic acid of synthetic iron and zinc taking zinc salt, molysite and oxalic acid as raw material solid phaseCompound.
5. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that the desulfurizing agent presoma of preparationDry at 80～130 DEG C.
6. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that the oxygen in described oxygen-containing atmosphereVolumetric concentration is 2～8%.
7. the method for preparing zinc ferrite desulfurization agent according to claim 1, is characterized in that described in-situ regeneration solidification processIn oxygen-containing atmosphere regeneration air speed be 2000～5000h-1。
CN201610916039.7A 2016-10-21 2016-10-21 Method for utilizing microwave in-situ synthesis to prepare zinc-ferrite desulfurizing agent Pending CN106336910A (en)

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Cited By (1)

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CN108905959A (en) * 2018-07-09 2018-11-30 太原理工大学 The method that microwave in-situ one-step method prepares ZnO/MCM-41 desulfurizing agent

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CN108905959A (en) * 2018-07-09 2018-11-30 太原理工大学 The method that microwave in-situ one-step method prepares ZnO/MCM-41 desulfurizing agent
CN108905959B (en) * 2018-07-09 2021-02-23 太原理工大学 Method for preparing ZnO/MCM-41 desulfurizer by microwave in-situ one-step method

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