CN101955193B - Method for preparing hydrogen and fertilizer ammonium sulfate by desulfurizing coal-fired waste gas - Google Patents

Method for preparing hydrogen and fertilizer ammonium sulfate by desulfurizing coal-fired waste gas Download PDF

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CN101955193B
CN101955193B CN2010102831228A CN201010283122A CN101955193B CN 101955193 B CN101955193 B CN 101955193B CN 2010102831228 A CN2010102831228 A CN 2010102831228A CN 201010283122 A CN201010283122 A CN 201010283122A CN 101955193 B CN101955193 B CN 101955193B
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ammonium
hydrogen
aqueous solution
ammonia
photocatalyst
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CN2010102831228A
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Chinese (zh)
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CN101955193A (en
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姚伟峰
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上海电力学院
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a method for preparing fuel hydrogen and an agricultural fertilizer ammonium sulfate from a coal-fired waste gas. The method comprises four steps of chemical adsorption of the coal-fired waste gas, forming of ammonium sulfate aqueous solution from an aerosol-state sub-ammonium salt, photo-catalytic reaction and product purification. Namely, on the basis of an ammonia desulfurization method, a photo-catalytic technique and an ammonia desulfurization technique are organically combined together to finish the conversion from the chemical adsorption of the coal-fired waste gas (sulfur dioxide) to the ammonium sulfate (the agricultural fertilizer ammonium sulfate) and the hydrogen (a new energy resource) with higher application value. Thus, the method reduces the operating expenses required by oxidation of the sub-ammonium salt during ammonia desulfurization, increases the product utility value, and has a higher application value.

Description

The method of a kind of coal combustion exhaust desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium

Technical field

The present invention relates to the method for a kind of coal combustion exhaust desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium ,Belonging to coal combustion exhaust handles and the developmental technology of new energy resources field.

Background technology

Environmental pollution and energy shortage are the significant challenge that current mankind faces, and also are that China implements the necessary top-priority key subjects of the strategy of sustainable development.The gaseous pollutant of industrial discharge is one of important source of topsoil, and wherein toxic harmful exhaust gas causes serious threat to human health and ecological security.Along with the fast development of industry such as China's electric power, the coal consumption amount increases substantially, and makes sulfur dioxide pollution constantly aggravate.China's sulphur dioxide emission occupy first place in the world at present, and surpass 2,000 ten thousand tons for years, and wherein power plant emission sulfurous gas accounts for 60% of total amount near 50%, two control district sulphur dioxide emission of total amount.China's acid rain and sulfur dioxide pollution are serious, and the acid rain area has accounted for 30% of area, and acid rain and sulfur dioxide pollution cause financial loss every year more than 1,000 hundred million yuan.Therefore, research and development is fit to China's national situation, and has the poisonous and harmful industrial waste gas purifying technology and equipment of independent intellectual property right, and exhaust gas utilization prepares new forms of energy and has important practical significance.

In recent years " ammonia process of desulfurization " because technology simple, front-end investment is few, the routine maintenance amount is little, desulfurization product is that chemical fertilizer advantages such as (ammonium fertilizer-ammonium sulfate) causes people's extensive concern.Its principle is to adopt ammoniacal liquor to contact mixing, the SO in the flue gas as desulfurization absorbent with the flue gas that gets into reaction tower 2Generate ammonium sulphite with the ammoniacal liquor reaction, again through at high temperature carrying out generating ammoniumsulphate soln after the oxidizing reaction with oxygen, through making chemical fertilizer ammonium sulfate after crystallization, dehydration, the press filtration, its sales revenue can be supported towards sweetening agent and working cost at last.Ammonia also is a kind of poisonous dusty gas, in synthetic ammonia or urea production process, can produce a large amount of ammonia-contaminated gas, itself just has the difficult problems that need to be resolved hurrily such as quantity discharged is big, pollution is heavy, hard to manage.The theory environmental pollution improvement work of the ammonia process of desulfurization this " with useless pollution treatment " " turning waste into wealth " has great importance.

Ammonia desulfurizing process is according to ammonia (NH 3) and sulfurous gas (SO 2), the water basic mechanism that is reacted into desulfurization product carries out, and mainly contains wet-type ammonia, electron beam ammonia process, impulse electric corona ammonia process, simple and easy ammonia process etc.Wherein wet-type ammonia is more sophisticated at present, industrialized ammonia desulfurizing process.The wet-type ammonia technological process generally is divided into three big steps: desulfurization absorption, intermediates are handled, the sub product manufacturing.Different according to process and by product, wet-type ammonia can be divided into ammonia-fertile method, ammonia-acid system, ammonia-ammonium sulfite etc. again.Wherein ammonia-fertile method is divided into fertile method of ammonia-ammonia sulfate and the fertile method of ammonia-ammonium phosphate again according to the product difference.The fertile method of ammonia-ammonia sulfate is a most popular method in the wet ammonia process desulfurizing technology.

The oxide treatment of the intermediates of the ammonia process of desulfurization-imonium salt is the key of decision ammonia desulfuration equipment economical operation, and methods such as pressure oxidation, catalyzed oxidation are arranged usually, all need build a cover oxidizer unit in addition, makes the working cost of total system be difficult to descend.Therefore development new technologies, ammonium sulphite bring great economic benefit will for enterprise and society to the required expense of the transformation of ammonium sulfate in the reduction ammonia process of desulfurization.

Photochemical catalysis can be converted into highdensity chemical energy, electric energy with low-density solar energy; Can directly utilize simultaneously in sunshine degraded and the mineralized water and airborne all contaminations; Through light-catalysed method; Making full use of the sunshine of cheapness and " green ", is an important channel that solves present global energy crisis and environmental pollution.Photocatalysis technology is comparatively extensive in the research of directions such as organic pollutant improvement and water decomposition hydrogen manufacturing, yet utilizes photochemical catalysis to carry out the research of coal combustion exhaust desulfurization, does not see relevant report both at home and abroad so far, does not also have related patent U.S. Patent No. to relate to this partial content.

Present patent application is on the basis of ammoniacal liquor doctor treatment, organically to combine photocatalysis technology and ammoniacal liquor desulfurization technology; The conversion of completion from the chemisorption of coal combustion exhaust (sulfurous gas) to ammonium sulfate with higher using value (agricultural fertilizer sulphur ammonium) and hydrogen (new forms of energy); Reduce in the ammonia process of desulfurization because of the required working cost of imonium salt oxidation; Increase product utilization and be worth, have higher application prospect.

Summary of the invention

The object of the present invention is to provide a kind of coal combustion exhaust (SO that utilizes 2) carry out utilization of waste material and prepare hydrogen and agricultural with the method for chemical fertilizer sulphur ammonium.

Know-why of the present invention

The present invention is a kind of technology of utilizing coal combustion exhaust to carry out photochemical catalysis desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium of on the basis of simple and easy ammoniacal liquor doctor treatment, developing.

Simple and easy ammonia process technology is simple; Working cost is cheap; But the desulfurization product major part of simple and easy ammonia process is the unsettled imonium salt of aerosol state, reclaims very difficulty, and its desulfurization product (unsettled imonium salt) decomposites sulfurous gas (SO with having part after the flue gas emptying again 2 ),Form secondary pollution.

Photochemical catalysis ammoniacal liquor method is organically to combine photocatalysis technology and ammonia process technology on the basis of simple and easy ammonia process; Utilize sun power to accomplish the conversion of (agriculture) and hydrogen (new forms of energy) with chemical fertilizer sulphur ammonium from waste gas (sulfurous gas) to ammonium sulfate with higher using value; Because of the required working cost of imonium salt oxidation, increase product utilization and be worth in the reduction ammonia process of desulfurization.

The main process of photochemical catalysis ammoniacal liquor method is carried out in two steps:

At first utilize the H under the gas phase condition 2O, NH 3With SO 2Between rapid reaction design easy reaction device carry out the ammonia process of desulfurization, its desulfurization product mainly is the unsettled imonium salt of aerosol state;

Make the product (imonium salt) of ammonia process of desulfurization step change into stable ammonium salt through light-catalysed step again and prepare hydrogen (new forms of energy) simultaneously with higher using value.

Technical scheme of the present invention

The method of a kind of coal combustion exhaust desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium, this method comprises the steps:

1. the chemisorption of coal combustion exhaust:

Sulfurous gas (SO in the coal combustion exhaust 2) and ammonia (NH 3) and water (H 2O) rapid reaction generates aerosol state imonium salt ((NH 4) 2SO 3);

2. the aerosol state imonium salt formation ammonium sulphite aqueous solution

At ammonia (NH 3) under the protective atmosphere, prepared aerosol state imonium the salt ((NH of step 1 4) 2SO 3) feed in the normal-temperature water, forming concentration is the ammonium sulphite aqueous solution of 0.1~6mol/L;

3. photochemical catalysis step

The ammonium sulphite aqueous solution of step 2 preparation; Be transferred to the light-catalyzed reaction chamber; Utilize high-activity photocatalyst (photocatalyst); Like Cadmium Sulfide photocatalysts such as (CdS), the ammonium sulphite aqueous solution is carried out solar irradiation, make the ammonium sulphite aqueous solution be finally converted into ammonium sulfate solution (product) and hydrogen (product) through the photochemical catalytic oxidation reduction reaction;

The reaction equation that is taken place is:

Photocatalyst (photocatalyst) is 0.09~0.2% of an ammonium sulphite aqueous solution weight like the consumption of Cadmium Sulfide photocatalysts such as (CdS).

4. product purification

The resulting product in step 3 reaction back comprises liquid ammonium sulfate solution and gasiform hydrogen;

Wherein gaseous product can be removed remaining ammonia to extract hydrogen after water filtration;

The ammonium sulfate solution that generates is through heating evaporation moisture, and chemical fertilizer sulphur ammonium is prepared in crystallization.

The photocatalyst of above-mentioned coal combustion exhaust desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium is solid particulate or film, and is reusable after filtering.

Beneficial effect of the present invention

The present invention is because the technical scheme that has adopted photochemical catalysis and ammoniacal liquor method to combine; Thereby has the effect of effectively removing coal combustion exhaust toxic pollutant and industrial ammonia pollutent; Simultaneously can also Hydrogen Energy be can be by conversion solar, hydrogen (new forms of energy) and chemical fertilizer sulphur ammonium prepared at last with higher using value.Utilize this technology can improve the product income that coal combustion exhaust is administered, reduce the cost that coal combustion exhaust is administered, have comparatively wide application prospect.

Description of drawings

Fig. 1, photochemical catalysis ammoniacal liquor method are handled the process flow diagram of coal combustion exhaust hydrogen manufacturing and chemical fertilizer sulphur ammonium.

Fig. 2, utilize Cadmium Sulfide CdS photocatalysis Decomposition (NH 4) 2SO 3Solution hydrogen manufacturing test.Reaction conditions: photocatalyst 0.5g CdS; Reaction solution 1M (NH 4) 2SO 3Solution 300ml; Light source: standard 1.5AM simulated solar irradiation (1000W xenon lamp), illuminating area 200 cm 2

Fig. 3, CdS photocatalysis Decomposition (NH 4) 2SO 3The endurance life test of solution hydrogen production activity.Reaction conditions: photocatalyst 0.5g CdS; Reaction solution 1M (NH 4) 2SO 3Solution 300ml; Light source: standard 1.5AM simulated solar irradiation (1000W xenon lamp), illuminating area 33 cm 2

Fig. 4, the ammonium sulphite aqueous solution chromatography of ions figure after light-catalyzed reaction.Test conditions: photocatalyst 0.5g CdS; Reaction solution 1M (NH 4) 2SO 3Solution 300ml; Light source: standard 1.5AM simulated solar irradiation (1000W xenon lamp), illuminating area 33 cm 2

Fig. 5, ammonium sulphite concentration of aqueous solution are to the influence of photocatalytic hydrogen production activity.Test conditions: photocatalyst 0.5g CdS; Reaction solution 1M (NH 4) 2SO 3Solution 300ml; Light source: standard 1.5AM simulated solar irradiation (1000W xenon lamp), illuminating area 33 cm 2

The consumption of Fig. 6, photocatalyst Cadmium Sulfide is to the influence of photocatalytic hydrogen production activity.Test conditions: photocatalyst CdS; Reaction solution 1M (NH 4) 2SO 3Solution 300ml; Light source: standard 1.5AM simulated solar irradiation (1000W xenon lamp), illuminating area 33 cm 2

Embodiment

Below through embodiment and combine accompanying drawing that the present invention is further set forth, but do not limit the present invention.

Utilize visible light catalytic material Cadmium Sulfide (CdS) to carry out the hydrogen manufacturing of coal combustion exhaust photochemical catalysis ammonia spirit desulfurization.Utilize ammoniacal liquor absorption sulfurous gas to generate ammonium sulfite solution, under the irradiation of simulated solar irradiation, utilize CdS to carry out the photochemical catalytic oxidation and the water decomposition hydrogen manufacturing of ammonium sulfite solution.The process flow diagram of concrete reaction is as shown in Figure 1:

Wherein ammoniacal liquor and the coal combustion exhaust combination generation sulfurous acid aqueous solution is had feasibility by ammoniacal liquor method proof, mainly illustrates for example here and uses the feasibility that photocatalysis technology makes sulfurous acid aqueous solution photochemical catalytic oxidation generation sulphur ammonium and hydrogen.

Starting material

Commercial Cadmium Sulfide (CdS); (0.5g purity 99.99%) (Alfa Aesar company)

Ammonium sulfite solution: (feeding ammoniacal liquor by sulfurous gas generates)

PdCl 2(purity 99.99%) (Aldrich company)

Cr (NO 3) 3(purity 98%) (Aldrich company)

NaBH 4, 98%, Acros Organics company

Polyvinlylpyrolidone (PVP, K30, average MW 40,000), Fluka company

Experimental procedure

The ammonium sulfite solution of configuration different concns: 0.1M, 0.3M, 0.35M, 0.5M, 1M, 3M, 6M;

Configuration light promotor Pd/Cr 2O 3:

The PdCl of configuration 1M 2And Cr (NO 3) 3The aqueous solution is pressed Pd:Cr 2O 3Mass ratio be that 4:1 mixes, add 0.03783g NaBH subsequently 4Pd/Cr is prepared in reduction 2O 3Light promoter metal colloidal sol adds 0.02g PVP and prevents that metal nanoparticle from precipitating because of reunion.

Photocatalysis hydrogen production and sulphur ammonium

Get the 300ml ammonium sulfite solution in photo catalysis reactor, add 0.5gCdS, under stirring state, add 2.5mgPd/Cr 2O 3The light promotor utilizes simulated solar irradiation (xenon lamp (1.5AM) Newport company) to carry out photocatalysis hydrogen production and the experiment of sulphur ammonium subsequently.

Catalyzed reaction result's experiment

Embodiment 1

The feasibility of photochemical catalytic oxidation reduction ammonium sulfite solution hydrogen manufacturing and chemical fertilizer sulphur ammonium

Fig. 2 is Cadmium Sulfide CdS photocatalysis Decomposition (NH 4) 2SO 3Solution hydrogen manufacturing test-results.As shown in Figure 2, the CdS that does not add promotor has possessed the ability of photocatalysis Decomposition ammonium sulfite solution, but hydrogen production activity is lower, and its hydrogen-producing speed has only 0.46 mL/min.

In concentration is the photocatalyst Cadmium Sulfide (CdS) that adds 0.5g in the ammonium sulphite aqueous solution of 1mol/L, adds photochemical catalysis promotor Pd/Cr simultaneously 2O 3Its result's contrast can find out that the photocatalytic activity of CdS is greatly improved; In photochemical catalysis promotor add-on is 0.5% o'clock of photocatalyst quality, and it goes out hydrogen speed and rises to 2.5ml/min fast, and this photo-quantum efficiency that is reflected in 350 to 520nm the light scope has reached 50%.Test-results shows that can reduce the mode of ammonium sulfite solution through photochemical catalytic oxidation makes hydrogen.

Embodiment 2

Photochemical catalytic oxidation reduction ammonium sulfite solution hydrogen production activity is stable

The reactive behavior that CdS photocatalysis Decomposition ammonium sulfite solution goes out hydrogen is comparatively stable.Fig. 3 shows the active endurance life test result who utilizes 0.5g photocatalyst Cadmium Sulfide (CdS) decomposition 1M ammonium sulphite aqueous solution hydrogen manufacturing test.As shown in the figure, CdS can keep the high reactivity non-stop run a few days, and the ammonium sulphite complete oxidation in solution is ammonium sulfate and prepares the hydrogen near 5 liters.This result shows and utilizes photocatalysis technology redox ammonium sulphite hydrogen manufacturing effectively, and can keep higher hydrogen manufacturing speed and the sun power effciency of energy transfer to Hydrogen Energy.

Embodiment 3

The thoroughness of photochemical catalytic oxidation reduction ammonium sulfite solution hydrogen manufacturing

But utilize light-catalysed method complete oxidation reduction ammonium sulfite solution; As shown in Figure 4; After the 1M ammonium sulfite solution is carried out the photocatalysis Decomposition hydrogen production reaction; Sulfite ion in the solution can be converted into sulfate ion fully, and this result shows and utilizes photocatalysis technology can realize the ammonium sulphite complete oxidation is generated ammonium sulfate and prepares the purpose of hydrogen.

Embodiment 4

Ammonium sulfite solution concentration is to the influence of photocatalytic hydrogen production activity

Research ammonium sulphite concentration of aqueous solution is to the active influence factor of photocatalytic hydrogen production by water decomposition.The ammonium sulphite aqueous solution of choosing concentration and be 0.1 mol to 6 mol saturation concentration is that reaction solution carries out the photocatalysis hydrogen production experiment.Fig. 5 shows that the concentration of the ammonium sulphite aqueous solution is bigger to the influence of photocatalytic hydrogen production activity, and when its concentration was in 0.5 mol to 6 mol, the hydrogen manufacturing of the photochemical catalysis ammonium sulphite aqueous solution was the highest to the utilising efficiency of sun power.

Embodiment5

The photocatalyst consumption is to the influence of photocatalytic hydrogen production activity

The consumption of photocatalyst has certain influence to photocatalytic hydrogen production activity.Fig. 6 has shown the influence of different amounts CdS photocatalyst to photocatalysis Decomposition ammonium sulfite solution hydrogen production activity.Experimental result show the consumption when Cadmium Sulfide (CdS) be ammonium sulphite aqueous solution weight 0.09~0.22% the time, catalyzer can show higher photocatalytic activity.

The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.。

Claims (3)

1. the method for coal combustion exhaust desulfurization hydrogen manufacturing and chemical fertilizer sulphur ammonium is characterized in that this method comprises the steps:
(1), the chemisorption of coal combustion exhaust:
Sulfurous gas (SO in the coal combustion exhaust 2) and ammonia (NH 3) and water (H 2O) rapid reaction generates aerosol state imonium salt (NH 4) 2SO 3
(2), the aerosol state imonium salt formation ammonium sulphite aqueous solution
With ammonia (NH 3) be protective atmosphere, the prepared aerosol state imonium salt (NH of step (1) 4) 2SO 3Feed in the normal-temperature water, forming concentration is the ammonium sulphite aqueous solution of 0.1~6mol/L;
(3), photochemical catalysis step
The ammonium sulphite aqueous solution of step (2) preparation; Be transferred to the light-catalyzed reaction chamber; Utilize the photocatalyst Cadmium Sulfide, the ammonium sulphite aqueous solution is carried out solar irradiation, make the ammonium sulphite aqueous solution be finally converted into ammonium sulfate solution and hydrogen through the photochemical catalytic oxidation reduction reaction;
The reaction equation that is taken place is:
The consumption of photocatalyst Cadmium Sulfide is 0.09~0.22% of an ammonium sulphite aqueous solution weight;
(4) product purification
The resulting product in step (3) reaction back comprises liquid ammonium sulfate solution and gasiform hydrogen; Wherein gaseous product is removed remaining ammonia and is extracted hydrogen after water filtration; The ammonium sulfate solution that generates is through heating evaporation moisture, and crystallization prepares chemical fertilizer sulphur ammonium.
2. the method for a kind of coal combustion exhaust desulfurization hydrogen manufacturing as claimed in claim 1 and chemical fertilizer sulphur ammonium is characterized in that, when adding the photocatalyst Cadmium Sulfide in the described photochemical catalysis step of step (3), adds the promotor Pd/Cr of photocatalyst Cadmium Sulfide 2O 3, its add-on is 0.5% of a photocatalyst Cadmium Sulfide weight.
3. the method for a kind of coal combustion exhaust desulfurization hydrogen manufacturing as claimed in claim 1 and chemical fertilizer sulphur ammonium; It is characterized in that; In the described aerosol state imonium of step (2) the salt formation ammonium sulphite aqueous solution step, the ammonium sulphite concentration of aqueous solution of formation is 0.5~6mol/L.
CN2010102831228A 2010-09-16 2010-09-16 Method for preparing hydrogen and fertilizer ammonium sulfate by desulfurizing coal-fired waste gas CN101955193B (en)

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CN105862063B (en) * 2016-06-02 2018-07-24 复旦大学 A method of the hydrogen manufacturing simultaneously of recovery processing sulfur dioxide

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CN101143291A (en) * 2006-09-13 2008-03-19 史选增 Low-consumption high-quality ammonium sulfate fertilizer recovery wet ammonia process desulfurizing technology
CN101543724A (en) * 2009-03-25 2009-09-30 南京东大苏威能源环保工程有限公司 Ammonia desulphurization method suitable for sintering flue gas treatment

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Publication number Priority date Publication date Assignee Title
US3676059A (en) * 1970-06-01 1972-07-11 Albert B Welty Jr Sulfate control in ammonia flue gas desulfurization
CN1843575A (en) * 2006-03-29 2006-10-11 华北电力大学 Method and apparatus for optic catalytic oxidizing, desulfurizing and denitrifying flue gas simultaneously
CN101143291A (en) * 2006-09-13 2008-03-19 史选增 Low-consumption high-quality ammonium sulfate fertilizer recovery wet ammonia process desulfurizing technology
CN101543724A (en) * 2009-03-25 2009-09-30 南京东大苏威能源环保工程有限公司 Ammonia desulphurization method suitable for sintering flue gas treatment

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