CN108624370B - Method for preparing biological methane by separating and purifying methane membrane - Google Patents
Method for preparing biological methane by separating and purifying methane membrane Download PDFInfo
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- CN108624370B CN108624370B CN201710164456.5A CN201710164456A CN108624370B CN 108624370 B CN108624370 B CN 108624370B CN 201710164456 A CN201710164456 A CN 201710164456A CN 108624370 B CN108624370 B CN 108624370B
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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
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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
- 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
Abstract
A process for preparing biomethane by membrane separation and purification of marsh gas includes such steps as preparing slurry from ardealite dregs, ammoniating, counter-current contact with marsh gas in membrane separator to absorb CO2And H2S, purifying the biogas to obtain the biological methane, and simultaneously by-producing the ammonium sulfate compound fertilizer and the calcium carbonate. Is particularly suitable for purifying the marsh gas prepared from various raw materials, and belongs to the technical field of carbon dioxide capture and utilization. The invention avoids the complicated gas pretreatment step required by a single membrane separation method, and realizes the resource utilization of CO by a separation-reaction one-step method2The purpose of treating waste by waste is achieved.
Description
Technical Field
A process method for preparing biological methane by methane membrane separation and purification belongs to the technical field of chemical separation, and particularly relates to the technical field of carbon dioxide capture and utilization.
Background
The biogas is combustible mixed gas generated by fermenting organic substances through various microorganism systems under anaerobic conditions, mainly comprises methane and carbon dioxide, and also contains a small amount of gases such as hydrogen, carbon monoxide, hydrogen sulfide, oxygen, nitrogen and the like. Generally speaking, CO in biogas2H content of 25-55% (mol)2The S content is 0.0006% -2%. The heat value of the untreated marsh gas is 20.16-28.98 MJ/Nm3The energy density is low, and the methane (CH) can only be used as a civil energy source for a long time499% -100%) of heat value is 38.22 MJ/Nm3It can be used as petroleum substitute for engine fuel. However, CO2、H2O and H2S severely corrodes equipment and piping, CO, during compression or during combustion for use as a vehicle fuel2And the methane number (combustion value) of the biogas is reduced, and for these two reasons, CO2、H2O、H2S must beIs removed before compression and reaches the standard of 'compressed natural gas for vehicles': CH (CH)4≥97%、CO2≤3%，H2S≤15 mg/m3。
The traditional concept of biogas purification is to separate acidic CO in biogas by methods of absorption, adsorption, membrane separation and the like2、H2S, making CH4The purity of (b) is improved to the corresponding standard. For example, the absorption method comprises introducing CO into an absorption tower with amine solvent such as MEA and DEA2Absorbing, then regenerating the solution, and recycling the regenerated solvent; the adsorption method is to adopt adsorbents such as molecular sieves and mesoporous materials to adsorb carbon dioxide in the biogas, then regenerate the adsorbents in a pressure swing or blowing mode, and recycle the regenerated adsorbents. The absorption and adsorption method has a disadvantage that a desulfurization treatment process is added before the operation because H2S not only poisons the adsorbent, but also makes the regeneration gas CO2The purity is reduced, which is not favorable for post-treatment. Containing high purity CO2The regeneration gas is further compressed before it can be stored for other use. The membrane separation method is to separate CO in the methane2、H2S selectively permeates the membrane, thereby enabling CH4The process of improved purity is of significant advantage since it is not recycled. However, the direct purification of biogas by membrane separation requires a complicated pretreatment process and contains CO in consideration of low purity and low pressure of acid gas at the permeate side2And H2The acid gas of S is difficult to apply.
Another idea for purifying the biogas is to purify a large amount of CO in the biogas2And a small amount of H2The S acid gas is directly utilized while being separated, and the mass transfer driving force is increased. For example, CN201410153531.4 proposes a method for co-producing nano calcium carbonate by biogas purification, in which lime milk slurry added with a dispersant is contacted with biogas in a membrane reactor, so as to obtain high-purity biomethane while purifying biogas, and obtain nano calcium carbonate with excellent performance. However, the prior patent does not mention H2The removal of S obviously needs to be carried out in advance, otherwise the quality of calcium carbonate is influenced.
Phosphogypsum is solid waste produced when phosphorite is treated by sulfuric acid in phosphoric acid productionSlag, the main component of which is calcium sulfate. 1 ton of phosphoric acid (in 100% P) is usually prepared2O5In terms of) 4.8 to 5.0 tons of phosphogypsum. The method is characterized in that the discharged phosphogypsum is about 2000 million tons every year in China, the accumulated discharge amount is nearly hundred million tons, the emission amount is the largest in gypsum waste residue, and the discharged phosphogypsum occupies a large amount of land to form a slag hill and seriously pollutes the environment. However, phosphogypsum is associated with CO in the presence of water2、NH3The following reactions occur:
2NH3 + CO2 + CaSO4·2H2O → CaCO3(fixed) ↓ + (NH)4）2SO4 + H2O
And H2S may also participate in the reaction:
2NH3 + H2S →（NH4）2S。
therefore, the idea of treating waste with waste can be considered, and the ammoniated phosphogypsum slurry is adopted to absorb CO in the biogas2And H2S, separation and utilization of CO2And H2S, the post-treatment step is omitted, and the calcium carbonate and ammonium sulfate compound fertilizer are co-produced. The invention aims at the requirement of simultaneously removing CO in the process of preparing the biological methane by methane purification2And H2The characteristic of S is that solid waste residue phosphogypsum is used, a membrane separator is used as a separation reaction platform, and the separated acid gas is fixedly utilized while the biogas is purified, so that the purpose of treating wastes with wastes is achieved.
Disclosure of Invention
The invention aims to provide a process method for preparing biomethane by membrane separation and purification of biogas, which adopts solid waste residue phosphogypsum and uses a membrane separator to separate CO in the biogas2And H2S is removed at the same time, thereby achieving the purposes of biogas purification, waste residue resource utilization and ammonium sulfate and calcium carbonate coproduction.
The invention is realized by the following steps: a process for preparing biomethane by membrane separation and purification of marsh gas features that the marsh gas containing acidic components (carbon dioxide and hydrogen sulfide) in raw marsh gas tank is reacted with the ardealite ammonia water solution from slurry pump in two-stage membrane separator in series, where ardealite slurry is preparedThe material is in the ammonia absorption reactor to absorb gas ammonia in a counter-current way, and the ammoniated phosphogypsum slurry is sent to a membrane separator by a conveying device; in the membrane separator, CO in the biogas2And H2S is transmitted to the slurry side of the membrane and reacts with phosphogypsum ammonia water to generate suspension of calcium carbonate and ammonium sulfate; the biogas is converted into biological methane after two-stage membrane separation and purification, and then is sent for use after gas-liquid separation, dehydration and deamination; absorb CO2And H2And (3) separating calcium carbonate by-products from the feed liquid of the S through solid-liquid separation, and crystallizing the liquid to obtain ammonium sulfate by-products.
Generally, the phosphogypsum slurry consists of phosphogypsum and water, wherein the mass percentage concentration of the phosphogypsum is 3% -15%.
The ammoniation process is a process of absorbing ammonia gas by adopting phosphogypsum slurry, and the ammoniated phosphogypsum slurry is phosphogypsum slurry absorbing ammonia.
The operation temperature of the ammoniation reactor is 0-10 ℃ so as to ensure the ammonia absorption effect of the phosphogypsum slurry.
The membrane separator membrane component is a hollow fiber membrane, the material is one of polypropylene, polytetrafluoroethylene, polyethylene, polyvinylidene fluoride and polyether sulfone, and the pore size of the membrane surface is 5-10 mu m.
The membrane separator is a shell-and-tube type, wherein gas passes through a tube pass of a fiber membrane, and phosphogypsum slurry passes through a shell pass of the membrane separator.
The membrane separator is in two-stage series connection, and the gas and the phosphogypsum slurry are in a countercurrent mass transfer process.
The operating pressure of the tube pass biogas of the membrane separator is 2-10 kPa, and the operating pressure of the shell pass phosphogypsum slurry is 15-40 kPa.
The advantages and the achieved effects of the invention are as follows: the solid waste residue phosphogypsum is adopted to absorb CO in the methane in a countercurrent way in a membrane separator after ammoniation2And H2S, converting the phosphogypsum into an ammonium sulfate compound fertilizer and calcium carbonate which can be recycled, and simultaneously purifying the biogas to obtain high-purity biomethane. Compared with the common membrane separation method, the method omits the pretreatment steps of compression, cooling filtration, desulfurization and the like, and simultaneously makes full use of useless components in the biogas to produceTo be available by-products. Compared with absorption and adsorption methods, the method omits the step of pre-desulfurization, does not need to consider the problem of regeneration, and has low operation and running cost. Is particularly suitable for purifying and purifying the biogas generated by fermenting various raw materials, can prepare high-purity biological methane, and realizes the purpose of treating wastes with processes of wastes against one another.
Drawings
FIG. 1 is a schematic diagram of the process flow of producing biomethane by membrane separation and purification of biogas in the embodiment.
In the figure, 1-biogas raw material gas storage tank, 2-primary membrane separator, 3-secondary membrane separator, 4-gas-liquid separator, 5-solid-liquid separator, 6-crystallizer, 7-dehydration and deammoniation reactor, 8-slurry pump, 9-ammonia absorption reactor, 10-CO2Sensor, 11-pH monitoring device.
Detailed Description
The invention is described in further detail below with reference to the figures and examples.
Referring to the attached drawing 1, the process of the following embodiment adopts solid waste phosphogypsum to prepare slurry with the mass percentage concentration of 3% -15%, and ammoniation treatment is carried out on the slurry in an ammonia absorption reactor, wherein the absorption temperature of ammonia is controlled to be 0-10 ℃ so as to ensure that the ammonia absorption capacity of the slurry is maximum. The ammoniated phosphogypsum slurry is pumped into a shell pass inlet of a secondary membrane separator by a slurry pump and simultaneously discharged from a shell pass outlet of the primary membrane separator, and the ammoniated phosphogypsum is purified and absorbed with CO in the secondary membrane separator2Absorption of CO in a primary membrane separator2And a small amount of H2And S. And (3) allowing the phosphogypsum slurry out of the primary membrane separator to enter a solid-liquid separator, fully settling and separating calcium carbonate and ammonium sulfate at the moment, allowing calcium carbonate to be obtained at the bottom of the solid-liquid separator, allowing an ammonium sulfate aqueous solution overflowing from the top of the solid-liquid separator to enter a crystallizer, evaporating water in the crystallizer and recycling, and directly using the crystallized ammonium sulfate as an ammonium sulfate compound fertilizer.
The marsh gas is led out from a marsh gas raw material gas storage tank and sequentially enters a primary membrane separator and a secondary membrane separator to be in countercurrent contact with the ammoniated phosphogypsum slurry, and CO in the marsh gas2And H2S is mostly removed in a first-stage membrane separator, and CO is carried out in a second-stage membrane separator2And deeply removing until the corresponding standard is reached. The biogas discharged from the secondary membrane separator is purified biomethane, enters a gas-liquid separator to separate water, then enters a dehydration and ammonia removal reactor to remove water and trace ammonia in the gas, and is discharged for use outside.
Example 1
Preparing phosphogypsum into an aqueous solution with the mass percentage concentration of 3 percent, adding the aqueous solution into an ammonia absorption reactor, injecting the aminated phosphogypsum slurry into a liquid inlet of a secondary membrane separator by a slurry pump, and keeping the liquid pressure at the inlet at 15 kPa. The membrane separator is made of polypropylene, and the pore diameter of the membrane surface is 5 mu m. The rest CO in the marsh gas is separated in a secondary membrane separator2Removing most of CO in the marsh gas in a first-stage membrane separator2And H2S is removed, then the carbonized phosphogypsum suspension slurry enters a solid-liquid separator, calcium carbonate is separated out from the bottom, the liquid at the top enters a crystallizer, a byproduct ammonium sulfate compound fertilizer is generated after crystallization, and water is recycled. After being led out from a methane raw material gas storage tank, the methane directly enters a primary membrane separator at the pressure of 2kPa to remove most of CO2And almost all of H2S, then enters a secondary membrane separator for further removing CO2The purified gas enters a gas-liquid separator, most of water is separated out, the gas enters a dehydration and deammoniation reactor, the purity of the dried biological methane can reach more than 97 percent, and CO is2The content is less than 3 percent.
Example 2
Preparing phosphogypsum into an aqueous solution with the mass percentage concentration of 9 percent, adding the aqueous solution into an ammonia absorption reactor, injecting the aminated phosphogypsum slurry into a liquid inlet of a secondary membrane separator by a slurry pump, and keeping the liquid pressure at the inlet at 25 kPa. The membrane separator is made of polytetrafluoroethylene, and the pore diameter of the membrane surface is 8 mu m. The rest CO in the marsh gas is separated in a secondary membrane separator2Removing most of CO in the marsh gas in a first-stage membrane separator2And H2S is removed, then the carbonized phosphogypsum suspension slurry enters a solid-liquid separator, calcium carbonate is separated out from the bottom, the liquid at the top enters a crystallizer, a byproduct ammonium sulfate compound fertilizer is generated after crystallization, and water is recycled. After the marsh gas is led out from the marsh gas raw material gas storage tank, the pressure is 6kPa, directly entering a first-stage membrane separator to remove most of CO2And almost all of H2S, then the obtained product enters a secondary membrane separator for further removing CO2, the purified gas enters a gas-liquid separator for separating most of water, and then enters a dehydration and deammoniation reactor, the purity of the dried biomethane can reach more than 98%, and the CO can reach more than 98%2The content is less than 2 percent.
Example 3
Preparing the phosphogypsum into a water solution with the mass percentage concentration of 15 percent, adding the water solution into an ammonia absorption reactor, injecting the aminated phosphogypsum slurry into a liquid inlet of a secondary membrane separator by a slurry pump, and keeping the liquid pressure at the inlet at 40 kPa. The membrane separator adopts polyether sulfone, and the pore diameter of the membrane surface is 10 mu m. The rest CO in the marsh gas is separated in a secondary membrane separator2Removing most of CO in the marsh gas in a first-stage membrane separator2And H2S is removed, then the carbonized phosphogypsum suspension slurry enters a solid-liquid separator, calcium carbonate is separated out from the bottom, the liquid at the top enters a crystallizer, a byproduct ammonium sulfate compound fertilizer is generated after crystallization, and water is recycled. After being led out from a methane raw material gas storage tank, the methane directly enters a primary membrane separator at the pressure of 10 kPa to remove most of CO2And almost all of H2S, then enters a secondary membrane separator for further removing CO2The purified gas enters a gas-liquid separator, most of water is separated out, the gas enters a dehydration and deammoniation reactor, the purity of the dried biological methane can reach more than 97 percent, and CO is2The content is less than 3 percent.
Example 4
Preparing phosphogypsum into an aqueous solution with the mass percentage concentration of 12 percent, adding the aqueous solution into an ammonia absorption reactor, injecting the aminated phosphogypsum slurry into a liquid inlet of a secondary membrane separator by a slurry pump, and keeping the liquid pressure at the inlet at 30 kPa. The membrane separator is made of polyvinylidene fluoride, and the pore diameter of the membrane surface is 7 mu m. The rest CO in the marsh gas is separated in a secondary membrane separator2Removing most of CO in the marsh gas in a first-stage membrane separator2And H2S is removed, then the carbonized phosphogypsum suspension slurry enters a solid-liquid separator, calcium carbonate is separated out from the bottom, the top liquid enters a crystallizer, and crystallization is carried out to generate raw materialsThe byproduct ammonium sulfate compound fertilizer is produced, and the water is recycled. After being led out from the methane raw material gas storage tank, the methane directly enters a primary membrane separator with the pressure of 8kPa to remove most of CO2And almost all of H2S, then the obtained product enters a secondary membrane separator for further removing CO2, the purified gas enters a gas-liquid separator for separating most of water, and then enters a dehydration and deammoniation reactor, the purity of the dried biomethane can reach more than 98%, and the CO can reach more than 98%2The content is less than 2 percent.
Claims (3)
1. A method for preparing biomethane by methane membrane separation and purification is characterized in that methane containing acidic components of carbon dioxide and hydrogen sulfide in a methane raw material gas storage tank reacts with phosphogypsum ammonia water solution from a slurry pump in a two-stage series membrane separator, wherein phosphogypsum slurry absorbs gas ammonia in an ammonia absorption reactor in a countercurrent mode, and ammoniated phosphogypsum slurry is conveyed to the membrane separator by conveying equipment; in the membrane separator, CO in the biogas2And H2S is transmitted to the slurry side of the membrane and reacts with phosphogypsum ammonia water to generate suspension of calcium carbonate and ammonium sulfate; the biogas is converted into biological methane after two-stage membrane separation and purification, and then is sent for use after gas-liquid separation, dehydration and deamination; absorb CO2And H2Separating calcium carbonate by-products from the feed liquid of S through solid-liquid separation, and crystallizing the liquid to obtain ammonium sulfate by-products;
the membrane separator membrane component is a hollow fiber membrane, the material is one of polypropylene, polytetrafluoroethylene, polyethylene, polyvinylidene fluoride and polyether sulfone, and the pore size of the membrane surface is 5-10 mu m; the membrane components in the membrane separator are connected in series in two stages, biogas passes through a fiber membrane tube pass, the phosphogypsum slurry passes through a fiber membrane shell pass, the pressure of the tube pass biogas in the membrane separator is 2-10 kPa, and the pressure of the shell pass phosphogypsum slurry is 15-40 kPa.
2. The method according to claim 1, characterized in that the phosphogypsum slurry is an emulsion formed by phosphogypsum and water, and the mass percentage concentration of the phosphogypsum is 3% -15%.
3. The method according to claim 1, wherein the temperature of the ammonia absorption reactor is controlled to be 0 to 10 ℃.
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| US20240117285A1 (en) | 2022-10-06 | 2024-04-11 | L'air Liquide, Societe Anonyme Pour L'etude Et L?Exploitation Des Procedes Georges Claude | Integrated system and method for methane production using off gas recycling to anaerobic digester from a gas separation membrane unit |
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