CN108624370A - The method that biogas UF membrane purifies biological methane processed - Google Patents
The method that biogas UF membrane purifies biological methane processed Download PDFInfo
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- CN108624370A CN108624370A CN201710164456.5A CN201710164456A CN108624370A CN 108624370 A CN108624370 A CN 108624370A CN 201710164456 A CN201710164456 A CN 201710164456A CN 108624370 A CN108624370 A CN 108624370A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/245—Preparation from compounds containing nitrogen and sulfur
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/548—Membrane- or permeation-treatment for separating fractions, components or impurities during preparation or upgrading of a fuel
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Treatment Of Sludge (AREA)
- Fertilizers (AREA)
- Processing Of Solid Wastes (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Biogas UF membrane purifies biological methane process processed, and slurry is prepared into using residue phosphogypsum, absorbs CO with biogas counter current contacting in membrane separator after ammonification2And H2S, biogas obtain purifying obtained biological methane, while by-product sulphur ammonium composite fertilizer and calcium carbonate.Particularly suitable for the purification of biogas made from various raw materials, belonging to collecting carbonic anhydride and utilizing technical field.The invention avoids the required cumbersome gas pre-treatment steps of single membrane separation process, realize separation reaction one-step method recycling CO2, achieved the purpose that the treatment of wastes with processes of wastes against one another.
Description
Technical field
Biogas UF membrane purifies biological methane process processed, belongs to technical field of chemical separation, and in particular to titanium dioxide
Carbon traps and utilizes technical field.
Background technology
Biogas is the burning mixture that organic substance is generated through the fermentation of multiple-microorganism system under anaerobic, mainly
Ingredient is methane and carbon dioxide, also contains the gases such as a small amount of hydrogen, carbon monoxide, hydrogen sulfide, oxygen, nitrogen.In general, in biogas
CO2Content is 25% ~ 55%（mol）, H2S contents are 0.0006% ~ 2%.Untreated biogas calorific value is in 20.16 ~ 28.98 MJ/
Nm3, energy density is low, can only be used for a long time as domestic energy, and biological methane（CH4Purity 99% ~ 100%）Calorific value
In 38.22 MJ/Nm3, can be used as oil substitutes and be directly used as engine fuel.However, CO2、H2O and H2S is in compression process
In or severe corrosion equipment and pipeline in as vehicle fuel combustion process, CO2The methane value of biogas is reduced again（Burning
Value）, in view of the two reasons, CO2、H2O、H2S must be removed before the compression, and reach China《Compressed natural gas used as vehicle fuel》's
Standard：CH4≥97%、CO2≤ 3%, H2S≤15 mg/m3。
The thinking of traditional methane purification is to go out the acid CO in biogas using the methods of absorption and sorption, UF membrane sub-argument2、
H2S makes CH4Purity improve to respective standard.Such as absorption process is to use MEA, DEA amine solvent, by CO in absorption tower2
It absorbs, then solution is made to regenerate, the solvent after regeneration recycles；Absorption method is using adsorbents such as molecular sieve, mesoporous materials
By the carbon dioxide adsorption in biogas, then make adsorbent reactivation by transformation or Purge methods, the sorbent circulation after regeneration
It uses.The shortcomings that absorption and absorption method is palpus increase desulfurization process process before operation, because of H2S not only poisons adsorbent, but also
Make regeneration gas CO2Purity reduces, and is unfavorable for post-processing.Contain high-purity CO2Regeneration gas need to pass through further compression could store with
It is used for other purposes.UF membrane rule is by the CO in biogas2、H2S selectively passes through film, to make CH4The method that purity improves, by
It has a clear superiority in without regeneration.However, complicated preprocessing process is needed using the direct purifying biogas of membrane separation process, and
In view of per-meate side sour gas purity is not high, pressure is relatively low, contain CO2And H2The more difficult application of sour gas of S.
Another thinking of methane purification is by a large amount of CO in biogas2And a small amount of H2S sour gas is straight while separation
It connects and is used, increase mass transfer force.As CN201410153531.4 proposes a kind of methane purification coproduction nano-calcium carbonate
Method, the milk of lime slurry that dispersant is added is contacted with biogas in membrane reactor, purifying marsh gas obtain high-purity life
While object methane, the nano-calcium carbonate of function admirable can be obtained.However, having patent does not refer to H2The place to go of S, it is clear that
It also needs to be removed in advance, otherwise influences the quality of calcium carbonate.
Ardealite be in phosphoric acid production with sulfuric acid treating phosphorite when the solid slag that generates, main component is calcium sulfate.
Usually produce 1 ton of phosphoric acid（With 100%P2O5Meter）Generate 4.8 ~ 5.0 tons of ardealites.About 20,000,000 tons of ardealite is discharged in China every year,
Accumulative nearly hundred million tons of discharge capacity, is maximum one kind of discharge capacity in gypsum offscum, and the ardealite of discharge occupies a large amount of soils, forms slag
Environment is seriously polluted on mountain.However, ardealite have water participation in the case of with CO2、NH3Following reaction occurs：
2NH3 + CO2 + CaSO4·2H2O → CaCO3（Gu）↓ + （NH4）2SO4 + H2O
And H2S can also participate in reacting：
2NH3 + H2S →（NH4）2S。
Therefore, the thinking using the treatment of wastes with processes of wastes against one another can be considered in we, is absorbed in biogas using the ardealite slurries of ammonification
CO2And H2S is detached and is utilized CO2With H2S eliminates post-processing step, while co-producing calcium carbonate and sulphur ammonium composite fertilizer.The present invention
It is to be needed for methane purification biological methane while removing CO2And H2The characteristic of S, using solid slag ardealite, with UF membrane
Device is that the sour gas isolated is fixed utilization, reach the treatment of wastes with processes of wastes against one another by separation reaction platform while purifying biogas
Purpose.
Invention content
It is useless using solid the purpose of the present invention is to provide the process that a kind of biogas UF membrane purifies biological methane processed
Slag ardealite, by the CO in biogas in membrane separator2And H2S is removed simultaneously, reaches methane purification, waste residue resource profit
With, the purpose of coproduction sulphur ammonium and calcium carbonate.
The invention is realized in this way：The method that biogas UF membrane purifies biological methane processed, it is characterised in that by biogas original
Expect in gas storage tank containing acidic components carbon dioxide, the biogas of hydrogen sulfide and the ardealite ammonia spirit from mashing pump in two-stage
It is reacted in series connection membrane separator, wherein ardealite slurry counter-current absorption gaseous ammonia, ardealite of ammonification in ammonia absorbing reaction device
Slurry is sent by conveying equipment to membrane separator；In membrane separator, the CO in biogas2And H2S transport is to the slurry side of film, with phosphorus
The reaction of gypsum ammonium hydroxide generates the suspension of calcium carbonate and ammonium sulfate；Biogas is converted into biological methane after the purification of two-stage UF membrane,
Again use is sent outside after gas-liquid separation and dehydration deamination；Absorb CO2And H2The feed liquid of S is through separating calcium carbonate by-product
Product obtain sulphur ammonium byproduct after liquid crystalization.
Usually, the ardealite slurry is made of ardealite and water, wherein the mass percentage concentration of ardealite be 3% ~
15%。
The ammonifying process refers to the process of absorbing ammonia using ardealite slurry, and the ardealite slurry of ammonification refers to absorbing
The ardealite slurry of ammonia.
The operation temperature of the ammoniation reactor is 0 ~ 10 DEG C, to ensure the suction ammonia effect of ardealite slurry.
The pattern of the membrane separator membrane module be hollow-fibre membrane, material be polypropylene, polytetrafluoroethylene (PTFE), polyethylene,
One kind in Kynoar, polyether sulfone, film surface pore size are 5 ~ 10 μm.
The membrane separator is shell-and-tube, and wherein gas walks the tube side of tunica fibrosa, and ardealite slurry walks the shell of membrane separator
Journey.
The membrane separator is two-stage series connection, and gas and ardealite slurry are countercurrent mass transfer process.
The operating pressure of the membrane separator tube side biogas is 2 ~ 10 kPa, and the operating pressure of shell side ardealite slurry is 15
~40 kPa。
Advantages of the present invention and the effect reached are：Using solid slag ardealite, after ammonification in membrane separator countercurrently
Absorb the CO in biogas2And H2S converts ardealite to the sulphur ammonium composite fertilizer and calcium carbonate that resourcebility utilizes, while biogas obtains
To purification, the biological methane of high-purity is obtained.Compared with common membrane separation process, it is pre- to eliminate compression, cold filtration, desulfurization etc.
Processing step, while the useless component in biogas is made full use of, generate available byproduct.Compared with absorption and sorption method, save
Pre- desulfurized step has been removed, without regeneration issues are considered, has operated and operating cost is low.Especially suitable for being given birth to various fermenting raw materials
At biogas purification, purification, the biological methane of high-purity can be made, realize the purpose of the treatment of wastes with processes of wastes against one another.
Description of the drawings
Fig. 1 is that embodiment biogas UF membrane purifies biological methane process flow diagram processed.
In figure, 1- marsh gas raw materials gas storage tanks, 2- level-one membrane separators, 3- two level membrane separators, 4- gas-liquid separators, 5- is solid
Liquid/gas separator, 6- crystallizers, 7- are dehydrated deamination reaction device, 8- mashing pumps, 9- ammonia absorbing reaction devices, 10-CO2Sensor, 11-
PH monitoring devices.
Specific implementation mode
The present invention is described in further detail with reference to the accompanying drawings and examples.
The technical process of following embodiment referring to attached drawing 1, use solid slag ardealite be configured to mass percentage concentration for
Slurry is carried out ammoniated treatment by 3% ~ 15% slurry in ammonia absorbing reaction device, and the absorption temperature for controlling ammonia is 0 ~ 10 DEG C, to protect
The ammonia absorbability for demonstrate,proving slurry is maximum.Ardealite slurry after ammonification is squeezed into the shell side import of two level membrane separator by mashing pump,
It is come out simultaneously from the shell-side outlet of level-one membrane separator, the ardealite after ammonification purifies in two level membrane separator absorbs CO2,
CO is absorbed in level-one membrane separator2With a small amount of H2S.The ardealite slurry for going out level-one membrane separator enters solid-liquid separator, calcium carbonate
Obtain sufficient sedimentation separation at this time with ammonium sulfate, solid-liquid separator bottom obtains calcium carbonate, and the sulphur ammonium that top overflow goes out is water-soluble
Liquid enters crystallizer, in a crystallizer reuse after moisture evaporation, and the ammonium sulfate crystallized out is used directly as sulphur ammonium composite fertilizer.
Biogas draws from marsh gas raw materials gas storage tank and sequentially enters level-one membrane separator and two level membrane separator, with ammonification
Ardealite slurry counter current contacting, the CO in biogas2And H2S is largely removed in level-one membrane separator, in two level membrane separator
Middle carry out CO2Deep removal is to reaching respective standard.The biogas for going out two level membrane separator is the biological methane after purification, into gas
Liquid/gas separator separates moisture, subsequently into dehydration deamination reaction device, removes the moisture and Ammonia in gas, submitting out-of-bounds makes
With.
Embodiment 1
Ardealite is configured to the aqueous solution that mass percentage concentration is 3%, ammonia absorbing reaction device, the ardealite slurry after ammonification is added
The liquid inlet of two level membrane separator is injected by mashing pump, holding Inlet fluid pressure is 15kPa.Membrane separator uses polypropylene
Material, film surface aperture are 5 μm.By remainder CO in biogas in two level membrane separator2It is removed, in level-one film point
From in device by major part CO in biogas2And H2S is removed, and the ardealite suspended nitride being then carbonized enters solid-liquid separator, bottom
Part separates out calcium carbonate, and overhead-liquid enters crystallizer, and by-product sulphur ammonium composite fertilizer, moisture reuse are generated after crystallization.Biogas is from natural pond
After gas raw material gas storage tank is drawn, pressure 2kPa is directly entered level-one membrane separator, removes most CO2And almost all
H2S further removes CO into secondary membrane separator afterwards2, purified gas enters gas-liquid separator, separates most of moisture
Afterwards, into dehydration deamination reaction device, the biological methane purity after drying is up to 97% or more, CO2Content is less than 3%.
Embodiment 2
Ardealite is configured to the aqueous solution that mass percentage concentration is 9%, ammonia absorbing reaction device, the ardealite slurry after ammonification is added
The liquid inlet of two level membrane separator is injected by mashing pump, holding Inlet fluid pressure is 25kPa.Membrane separator uses polytetrafluoro
Ethylene material, film surface aperture are 8 μm.By remainder CO in biogas in two level membrane separator2It is removed, in level-one
By major part CO in biogas in membrane separator2And H2S is removed, and the ardealite suspended nitride being then carbonized enters separation of solid and liquid
Calcium carbonate is isolated in device, bottom, and overhead-liquid enters crystallizer, and by-product sulphur ammonium composite fertilizer, moisture reuse are generated after crystallization.Biogas
From after the extraction of marsh gas raw materials gas storage tank, pressure 6kPa is directly entered level-one membrane separator, removes most CO2Almost
Whole H2S, enters the further emergence work of secondary membrane separator afterwards, and purified gas enters gas-liquid separator, separates major part
After moisture, into dehydration deamination reaction device, the biological methane purity after drying is up to 98% or more, CO2Content is less than 2%.
Embodiment 3
Ardealite is configured to the aqueous solution that mass percentage concentration is 15%, ammonia absorbing reaction device is added, the ardealite slurry after ammonification
Material is injected the liquid inlet of two level membrane separator by mashing pump, and holding Inlet fluid pressure is 40 kPa.Membrane separator is using poly-
Ether sulfone, film surface aperture are 10 μm.By remainder CO in biogas in two level membrane separator2It is removed, in level-one film point
From in device by major part CO in biogas2And H2S is removed, and the ardealite suspended nitride being then carbonized enters solid-liquid separator, bottom
Part separates out calcium carbonate, and overhead-liquid enters crystallizer, and by-product sulphur ammonium composite fertilizer, moisture reuse are generated after crystallization.Biogas is from natural pond
After gas raw material gas storage tank is drawn, pressure is 10 kPa, is directly entered level-one membrane separator, removes most CO2It is almost complete
Portion H2S further removes CO into secondary membrane separator afterwards2, purified gas enters gas-liquid separator, separates most of water
After point, into dehydration deamination reaction device, the biological methane purity after drying is up to 97% or more, CO2Content is less than 3%.
Embodiment 4
Ardealite is configured to the aqueous solution that mass percentage concentration is 12%, ammonia absorbing reaction device is added, the ardealite slurry after ammonification
Material is injected the liquid inlet of two level membrane separator by mashing pump, and holding Inlet fluid pressure is 30 kPa.Membrane separator is using poly-
Vinylidene material, film surface aperture are 7 μm.By remainder CO in biogas in two level membrane separator2It is removed,
By major part CO in biogas in level-one membrane separator2And H2S is removed, and the ardealite suspended nitride being then carbonized enters solid-liquid
Calcium carbonate is isolated in separator, bottom, and overhead-liquid enters crystallizer, and by-product sulphur ammonium composite fertilizer, moisture reuse are generated after crystallization.
For biogas from after the extraction of marsh gas raw materials gas storage tank, pressure 8kPa is directly entered level-one membrane separator, removes most CO2With
Almost all H2S enters the further emergence work of secondary membrane separator afterwards, and purified gas enters gas-liquid separator, separates big
After partial moisture, into dehydration deamination reaction device, the biological methane purity after drying is up to 98% or more, CO2Content is less than 2%.
Claims (6)
1. the method that biogas UF membrane purifies biological methane processed, it is characterised in that acidic components will be contained in marsh gas raw materials gas storage tank
Carbon dioxide, hydrogen sulfide biogas reacted in two-stage series connection membrane separator with the ardealite ammonia spirit from mashing pump,
The ardealite slurry of middle ardealite slurry counter-current absorption gaseous ammonia in ammonia absorbing reaction device, ammonification is sent by conveying equipment to film point
From device；In membrane separator, the CO in biogas2And H2S transport reacts with ardealite ammonium hydroxide to the slurry side of film and generates calcium carbonate
With the suspension of ammonium sulfate；Biogas is converted into biological methane after the purification of two-stage UF membrane, then through gas-liquid separation and dehydration deamination
After send use outside；Absorb CO2And H2The feed liquid of S obtains sulphur ammonium pair through separating calcium carbonate byproduct after liquid crystalization
Product.
2. according to the method described in claim 1, it is characterized in that ardealite slurry is the emulsion formed by ardealite and water
The mass percentage concentration of body, ardealite is 3% ~ 15%.
3. according to the method described in claim 1, it is characterized in that ammonia absorbing reaction device controlled at 0 ~ 10 DEG C.
4. according to the method described in claim 1, it is characterized in that membrane separator membrane module pattern is hollow-fibre membrane, material is
One kind in polypropylene, polytetrafluoroethylene (PTFE), polyethylene, Kynoar, polyether sulfone, film surface pore size are 5 ~ 10 μm.
5. according to the method described in claim 1, it is characterized in that the membrane module in membrane separator is two-stage series connection, biogas walks fibre
Membrane tube journey is tieed up, ardealite slurry walks tunica fibrosa shell side.
6. according to the method described in claim 5, it is characterized in that the pressure of tube side biogas is 2 ~ 10 kPa, shell in membrane separator
The pressure of journey ardealite slurry is 15 ~ 40 kPa.
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Cited By (2)
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| CN113522007A (en) * | 2021-07-30 | 2021-10-22 | 哈尔滨工业大学 | Double-membrane aeration membrane biofilm reactor for biogas purification and use method thereof |
| EP4349455A1 (en) | 2022-10-06 | 2024-04-10 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Improved integrated system and method for methane production using off gas recycling to anaerobic digester from a gas separation membrane unit |
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| EP4349455A1 (en) | 2022-10-06 | 2024-04-10 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Improved integrated system and method for methane production using off gas recycling to anaerobic digester from a gas separation membrane unit |
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