WO2016082269A1 - Procédé de préparation de biométhane par purification de biogaz - Google Patents

Procédé de préparation de biométhane par purification de biogaz Download PDF

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WO2016082269A1
WO2016082269A1 PCT/CN2014/094784 CN2014094784W WO2016082269A1 WO 2016082269 A1 WO2016082269 A1 WO 2016082269A1 CN 2014094784 W CN2014094784 W CN 2014094784W WO 2016082269 A1 WO2016082269 A1 WO 2016082269A1
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absorbent
biogas
tank
absorption tower
mpa
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PCT/CN2014/094784
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English (en)
Chinese (zh)
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杨祝红
丁键
陈义峰
李峥
马春燕
刘畅
陆小华
谢瑞杰
袁圣娟
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南京工业大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • 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

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  • the invention belongs to the field of gas separation, and relates to a method for purifying and purifying biogas to prepare biomethane, in particular to using a choline eutectic solvent or at least one of an imidazole ionic liquid as an active ingredient to purify and purify biogas to prepare a living organism.
  • the method of methane is not limited to methane.
  • Biogas is a safe, clean and renewable energy source. Its main component is methane, about 45-60%, carbon dioxide, about 40-55%, and a small amount of water, hydrogen sulfide, nitrogen, oxygen and other trace gases. Biogas can be obtained by anaerobic fermentation of poor biomass (straw, human and animal waste, domestic garbage, etc.). Biogas can be obtained by purifying and purifying biogas (methane content is more than 97%), which can be widely used in vehicles. The use of energy, chemical raw materials, etc., is an important means to improve China's energy structure and solve environmental problems.
  • the biogas purification technologies widely used at present are mainly water washing method, alcohol amine method and membrane separation.
  • the equipment cost of the water washing method is too high, and the microorganisms in the absorption tower are easy to breed microorganisms; the energy consumption of the absorbent of the alcohol amine method is higher, and the corrosion of the equipment is also serious; the methane loss of the membrane separation method is relatively large, and the requirements for the preliminary treatment are required. High and large-scale have certain technical difficulties.
  • Chinese patent application CN104083989 A discloses a method for purifying and purifying biogas pressure water, the main equipments are: a pressurizing device, a buffer tank, a water washing tower, a analytical tower, a dryer, and the method utilizes the solubility of carbon dioxide, hydrogen sulfide and methane in water.
  • a water washing tower is constructed according to a physical adsorption process, and carbon dioxide and hydrogen sulfide gas in the biogas are removed by pressure water washing. The absorption efficiency is not high, and the investment in equipment after industrial amplification is large.
  • Chinese patent application CN102059037 A discloses a process for purifying carbon dioxide from natural gas tail gas, using MEA (ethanolamine) lean liquid to absorb carbon dioxide, and then releasing carbon dioxide, converting carbon dioxide in tail gas into liquid carbon dioxide for industrial production. .
  • MEA ethanolamine
  • the regeneration energy consumption of the absorbent in the method is high.
  • the object of the present invention is to provide a method for purifying and purifying biogas to produce biomethane, which has the advantages of high cost of the water washing method and high energy consumption of the alcohol amine method absorbent regeneration in the prior art, and the method can improve the absorption effect while improving the absorption effect. Reduce the regeneration energy consumption of the absorbent, thereby reducing the overall biomethane production cost.
  • a method for purifying and purifying biogas to prepare biomethane comprises the following steps:
  • the biogas is pressurized to 0.3 MPa to 20 MPa;
  • the pressure in the absorption tower is 0.3 MPa to 20 MPa, and the ratio of the flow rate of the absorbent to the biogas is 8 to 100 kg/h: 1 Nm 3 /h;
  • the absorbent is a choline eutectic solvent Or an aqueous solution containing at least one of an imidazole-based ionic liquid as an active ingredient, wherein the mass fraction of the active ingredient in the absorbent is from 5 to 90%.
  • the absorbent which absorbs carbon dioxide in step (2) enters a flash tank for regeneration treatment, and the pressure in the flash tank is 0.2-0.5 MPa, and the temperature is normal temperature (15).
  • the step (1) according to the content of hydrogen sulfide in the biogas, it is determined whether the hydrogen sulfide removal treatment needs to be performed first.
  • the content of hydrogen sulfide in the biogas is ⁇ 80 ppm
  • the biogas is removed after the hydrogen sulfide treatment in the desulfurization tower.
  • the pressurization system is pressurized; when the content of hydrogen sulfide in the biogas is ⁇ 80 ppm, the biogas is directly pressurized by the pressurization system.
  • the temperature in the absorption tower is normal temperature (15 to 30 ° C); the pressure in the absorption tower is preferably 0.6 MPa to 2 MPa, further preferably 1.2 MPa to 2 MPa;
  • the ratio of the flow rate of the agent to the biogas is preferably 15 to 40 kg/h: 1 Nm 3 /h, and more preferably 15 to 30 kg/h: 1 Nm 3 /h.
  • the mass fraction of the active ingredient in the absorbent is preferably from 15% to 50%.
  • the active ingredient of the absorbent is at least one of a choline eutectic solvent or an imidazole ionic liquid; the mass ratio of the choline eutectic solvent to the imidazole ionic liquid in the absorbent is 1: 0 to 4.
  • the choline eutectic solvent is A Formed after mixing with B, A is ChCl (choline chloride), [Choline] [Pro] (choline valine), [Choline] [Gly] (choline glycine), [Choline] [Ala] (biliary One of [alkaline alanine), [Choline] [Lys] (choline lysine), and B is at least one of urea (urea), EG (ethylene glycol) or PEG (polyethylene glycol) The molar ratio
  • the methane finished gas has CH 4 ⁇ 95%, CO 2 ⁇ 4%, and H 2 S ⁇ 40 ppm.
  • the invention also provides a system for purifying and purifying biogas to prepare biomethane, comprising: desulfurization tank, gas-liquid separation tank I, pressurization system, buffer tank, absorption tower, flash tank, analytical tower, absorbent circulating pump , absorbent tank, gas and liquid
  • the tank I and the drying tank are connected; the outlet of the desulfurization tank is connected to the inlet of the gas-liquid separation tank I, and the outlet of the gas-liquid separation tank I is connected to the inlet of the lower portion of the buffer tank via a pressurization system, the buffer The outlet of the upper part of the tank is connected with the inlet of the lower part of the absorption tower, and the upper part of the absorption tower is provided with at least one layer of nozzles, and the outlet of the top of the absorption tower is connected with the methane collecting device through the gas-liquid separation tank I and the drying tank; the absorption The liquid outlet at the bottom of the tower is connected to the absorbent inlet of the flash tank, the liquid outlet at the bottom of the flash
  • the system for purifying and purifying biogas to produce biomethane has at least two parallel dryers.
  • the upper part of the absorption tower is provided with at least one layer of nozzle for spraying the absorbent; the top of the absorption tower is provided with a mist eliminator; and the biogas inlet line of the absorption tower section is provided with a check valve, and the absorption liquid in the absorption tower is introduced into the liquid
  • a fine adjustment valve is arranged on the pipeline; a liquid outlet at the bottom of the absorption tower is provided with a regulating valve; and an exhaust valve is arranged at an air outlet of the absorption tower.
  • the top of the flash tank is provided with an air outlet and an exhaust port, and the flash tank is connected to the inlet of the gas-liquid separation tank I through an air outlet, and a check valve is arranged on the air outlet of the flash tank, and the flash tank is provided.
  • the exhaust port is provided with an exhaust valve for exhausting the air.
  • the liquid outlet line at the bottom of the flash tank and the other liquid outlet line at the lower part of the flash tank are each provided with a one-way valve.
  • the invention adopts a method for purifying and purifying biomethane by purifying biogas, and uses an ionic liquid (choline eutectic solvent, imidazole ionic liquid) aqueous solution as an absorbent, and the ionic liquid has good stability and greatly dissolves the gas. It can effectively remove carbon dioxide and hydrogen sulfide gas from biogas, and the purity of methane in the obtained product gas can reach 95%.
  • the absorbent can be regenerated, the regeneration efficiency is over 95%, the energy consumption of the absorbent is low, the equipment is easy to operate, and the investment is low.
  • Figure 1 is a system for purifying and purifying biogas to prepare biomethane
  • FIG. 1 1-desulfurization tower, 2-gas liquid separation tank I, 3-pressurization system, 4-buffer tank, 5-absorption tower, 6-flash tank, 7-analysis tower, 8-absorption and circulation pump , 9-absorbent storage tank, 10-gas liquid separation tank II, 11 - drying tank I, 12 - drying tank II.
  • Figure 2 shows the effect of the pressure in the absorption tower and the content of the active ingredient in the absorbent on the preparation of biomethane.
  • Figure 3 is a graph showing the effect of the ratio of the flow rate of the absorbent to the biogas on the preparation of biomethane.
  • a system for purifying and purifying biogas to prepare biomethane includes: desulfurization tank 1, gas-liquid separation tank I2, pressurization system 3, buffer tank 4, absorption tower 5, flash tank 6, and analysis a tower 7, an absorbent circulation pump 8, an absorbent tank 9, a gas-liquid separation tank I10, and a drying tank;
  • the outlet of the desulfurization tank 1 is connected to the inlet of the gas-liquid separation tank I2, and the gas-liquid separation tank I2
  • the outlet is connected to the inlet of the lower portion of the buffer tank 4 via the pressurization system 3, the outlet of the upper portion of the buffer tank 4 is connected to the inlet of the lower portion of the absorption tower 5, and the upper portion of the absorption tower is provided with at least one layer of nozzles, and the absorption tower 5
  • the gas outlet of the top is connected by a gas-liquid separation tank I10, two parallel drying tanks I11, a drying tank II12 and a methane collecting device; the liquid outlet at the bottom of the absorption tower 5 is connected
  • the upper part of the absorption tower 5 is provided with at least one layer of nozzles for spraying the absorbent; the top of the absorption tower 5 is provided with a mist eliminator; and the biogas inlet line of the absorption tower 5 is provided with a check valve for absorption in the absorption tower 5
  • a liquid regulating valve is provided on the liquid inlet pipe; a liquid outlet at the bottom of the absorption tower 5 is provided with a regulating valve; and an exhaust valve is arranged at an air outlet of the absorption tower 5.
  • the liquid outlet line at the bottom of the flash tank 6 and the other liquid outlet line at the lower portion of the flash tank 6 are each provided with a check valve.
  • the top of the flash tank 6 is provided with an air outlet and an exhaust port, and the flash tank 6 is connected to the inlet of the gas-liquid separation tank I2 via an air outlet, and a check valve is arranged on the air outlet of the flash tank 6.
  • the exhaust port of the flash tank 6 is provided with an exhaust valve for exhausting the air.
  • the biogas output from the biogas storage tank determines whether it needs to be removed from the desulfurization tank 1 according to the hydrogen sulfide content, and the biogas is pressurized to 0.3 MPa to 20 MPa by the pressurization system 3, and then passed through the buffer tank 4 and the self-absorption tower 5
  • the lower part of the inlet into the absorption tower 5 to the pressure in the tower reaches 0.3 MPa to 20 MPa, and then the biogas is continuously introduced, and the absorbent is sprayed into the tower through the nozzle at the upper part of the absorption tower 5, in which the pressure in the tower is maintained.
  • the biogas is fully contacted with the absorbent to remove carbon dioxide in the biogas, and the carbon dioxide-removing gas is taken from the gas outlet of the top of the absorption tower 5 through the gas-liquid separation tank I10 and two parallel drying tanks.
  • the absorbent that absorbs carbon dioxide is sent from the liquid outlet at the bottom of the absorption tower 5 to the flash tank 6 (pressure is 0.2-0.5 MPa, temperature is 15-30 °C) performing regeneration treatment, when the pressure difference between the pressure of the absorption tower 5 and the flash tank 6 is ⁇ 0.5 MPa, the absorbent which absorbs carbon dioxide is regenerated in the flash tank 6 to remove carbon dioxide; when the pressure and flash of the absorption tower 5 When the pressure difference of the tank 6 is ⁇ 0.5 MPa, the absorbent which has absorbed carbon dioxide is regenerated in the flash tank 6, and then enters the analysis tower 7 for thermal regeneration treatment to remove carbon dioxide, wherein the pressure in the analytical column 7 is 0.1 MPa, and the temperature is 50. ⁇ 95 ° C.
  • the regenerated treatment absorbent is sent to the absorbent tank 9 and sent to the absorption tower 5 by the absorbent circulation pump 8.
  • Biogas (methane 55.1%, carbon dioxide 44.6%, hydrogen sulfide 2547ppm) was removed from the sulfurization tank 1 by hydrogen sulfide, and the hydrogen sulfide-removing biogas (methane 55.1%, carbon dioxide 44.6%, hydrogen sulfide 83 ppm) was pressurized by the pressurization system 3 to 0.8MPa, the pressurized biogas is passed into the absorption tower 5 from the lower part of the absorption tower 5 through the buffer tank 4 at a flow rate of 5Nm 3 /h until the pressure in the tower reaches 0.8 MPa, and then the biogas is continuously introduced at the same flow rate, and at the same time
  • the absorbent (5% by weight of choline chloride and urea solution, choline chloride and urea in a molar ratio of 1:2) is delivered to the absorption tower 5 at a flow rate of 100 kg/h, and is sprayed from the nozzle in the upper part of the column.
  • the pressure in the tower is maintained at 0.8 MPa, the temperature is 25 to 30 ° C, the biogas is sufficiently contacted with the absorbent to remove carbon dioxide in the biogas, and the carbon dioxide-removing gas is dried to obtain the bio-methane product gas, to the living organism.
  • Component analysis of methane product gas is performed in the tower.
  • the absorbent from the bottom of the absorption tower 5 is analyzed and regenerated by a flash tank 6 (pressure: 0.4 MPa, temperature: 25 to 30 ° C), and an analytical tower 7 (pressure: 0.1 MPa, temperature: 70 ° C), and the regenerated absorbent is transported to the absorption.
  • the agent tank 9 is reused, and the absorbent regeneration efficiency is 95% or more.
  • the internal pressure has little effect on the methane content.
  • the pressure in the absorption tower is 0.8-2.0 MPa, especially 1.2 MPa-2.0 MPa
  • the biogas is purified and purified by using an absorbent having a mass fraction of 15% to 50%, and CH 4 ⁇ 95 can be obtained.
  • the biogas flow rate is 4Nm 3 /h
  • the absorption pressure in the absorption tower is 1MPa
  • the mass fraction is 30% of the absorbent (choline chloride and urea aqueous solution, the molar ratio of choline chloride to urea is 1:2), other conditions and
  • the effects of the absorbent flow rates of 40 kg/h, 60 kg/h, 80 kg/h, 100 kg/h, 120 kg/h, 150 kg/h, and 160 kg/h on the preparation of biomethane were examined.
  • the biogas is purified by using an absorbent with a mass fraction of 30%, when the flow rate of the absorbent is 40-160 kg/h, along with the flow rate of the absorbent.
  • the methane content in the methane product gas increases accordingly, and when the absorbent flow rate is 60-160 kg/h (the ratio of the absorbent flow rate to the biogas flow rate is 15 to 40 kg/h: 1 Nm 3 /h), the methane content is Above 95%, but when the absorbent flow rate reaches 120 kg / h (the ratio of the absorbent flow rate to the biogas flow rate is 30 kg / h: 1 Nm 3 / h), the methane content does not change much as the flow rate of the absorbent increases.
  • Biogas (methane 55.1%, carbon dioxide 44.6%, hydrogen sulfide 2396ppm) was removed from the sulfurization tank 1 by hydrogen sulfide, and the hydrogen sulfide-removing biogas (methane 55.1%, carbon dioxide 44.6%, hydrogen sulfide 76 ppm) was pressurized by the pressurization system 3 to 0.8MPa, the pressurized biogas is passed into the absorption tower 5 from the lower part of the absorption tower 5 through the buffer tank 4 at a flow rate of 3Nm 3 /h until the pressure in the tower reaches 0.8 MPa, and then the biogas is continuously introduced at the same flow rate, and at the same time Absorbent (25% by mass of ChCl+urea+[Cmim][Br], the molar ratio of ChCl to urea is 1:1.5, [Cmim][Br] is 20% of the absorbent) to 50kg/h The flow rate is sent to the absorption tower 5, and is sprayed into the tower by
  • the pressure in the tower is maintained at 0.8 MPa, and the temperature is 25 to 30 ° C, so that the biogas is sufficiently contacted with the absorbent to remove the biogas.
  • Carbon dioxide, the carbon dioxide-removing gas is dried to obtain a bio-methane product gas, and the bio-methane product gas is subjected to component analysis, and the methane content is 95.7%, carbon dioxide is 3.4%, and hydrogen sulfide is 34 ppm.
  • the absorbent from the bottom of the absorption tower 5 is regenerated and regenerated by a flash tank 6 (pressure 0.35 MPa, temperature 25 to 30 ° C), analytical column 7 (pressure 0.1 MPa, temperature 80 ° C), and the regenerated absorbent is transported to the absorption.
  • the agent tank 9 is reused, and the absorbent regeneration efficiency is 95.5%.
  • Biogas (55.3% of methane, 44.7% of carbon dioxide, 2254ppm of hydrogen sulfide) is desulfurized by desulfurization tank 1 to remove hydrogen sulfide.
  • the biogas from which hydrogen sulfide is removed (55.3% of methane, 44.7% of carbon dioxide, 84ppm of hydrogen sulfide) is pressurized by the pressurization system 3.
  • the pressurized biogas is passed into the absorption tower 5 from the lower part of the absorption tower 5 through the buffer tank 4 at a flow rate of 6Nm 3 /h until the pressure in the tower reaches 1.2 MPa, and then the biogas is continuously introduced at the same flow rate, and at the same time
  • Absorbent (20% by mass of ChCl+urea+[Cmim][BF 4 ] aqueous solution, the molar ratio of ChCl to urea is 1:2, [Cmim][BF 4 ] accounts for 15% of the absorbent mass) to 90kg
  • the flow rate of /h is sent to the absorption tower 5, and is sprayed into the tower from the nozzle in the upper part of the tower.
  • the pressure in the tower is maintained at 1.2 MPa, the temperature is 15-20 ° C, and the biogas is sufficiently contacted with the absorbent to remove the biogas.
  • the carbon dioxide in the carbon dioxide gas is dried to obtain the biomethane product gas, and the biomethane product gas is subjected to component analysis, and the methane content is 95.3%, the carbon dioxide is 3.8%, and the hydrogen sulfide is 35 ppm.
  • the absorbent from the bottom of the absorption tower 5 is regenerated by a flash tank 6 (pressure: 0.4 MPa, temperature: 15 to 20 ° C), and the regenerated absorbent is sent to the absorbent tank 9 for reuse, and the absorbent regeneration efficiency is 95.6%.
  • Biogas (methane 55.4%, carbon dioxide 44.2%, hydrogen sulfide 2365ppm) is removed from the sulfurization tank 1 by hydrogen sulfide, and the hydrogen sulfide-removing biogas (methane 55.4%, carbon dioxide 44.2%, hydrogen sulfide 79ppm) is pressurized by the pressurization system 3 to 1.2MPa, the pressurized biogas is passed into the absorption tower 5 from the lower part of the absorption tower 5 through the buffer tank 4 at a flow rate of 5Nm 3 /h until the pressure in the tower reaches 1.2 MPa, and then the biogas is continuously introduced at the same flow rate, and at the same time
  • the absorbent (30% by mass of ChCl+urea+EG aqueous solution, ChCl, urea and EG molar ratio of 1:1.5:0.5) is sent to the absorption tower 5 at a flow rate of 100 kg/h, and sprayed on the tower from the nozzle in the upper part of the tower.
  • the pressure in the tower is maintained at 1.2 MPa, the temperature is 20-25 ° C, the biogas is sufficiently contacted with the absorbent to remove carbon dioxide in the biogas, and the carbon dioxide-removed gas is dried to obtain the bio-methane product gas, and the bio-methane is produced.
  • the finished gas was analyzed for composition, with a methane content of 95.5%, a carbon dioxide content of 3.9%, and a hydrogen sulfide content of 36 ppm.
  • the absorbent from the bottom of the absorption tower 5 is regenerated by the flash tank 6 (pressure 0.4 Mpa, temperature 20-25 ° C), and the regenerated absorbent is transferred to the absorbent tank 9 for reuse.
  • the absorbent regeneration efficiency is 96.1. %.
  • Biogas (55.6% of methane, 44.5% of carbon dioxide, 2459ppm of hydrogen sulfide) is removed from the hydrogen sulfide by the desulfurization tank 1, and the biogas from which hydrogen sulfide is removed (55.6% of methane, 44.5% of carbon dioxide, and 85 ppm of hydrogen sulfide) is pressurized by the pressurization system 3.
  • the pressurized biogas is passed into the absorption tower 5 from the lower part of the absorption tower 5 through the buffer tank 4 at a flow rate of 5Nm 3 /h until the pressure in the tower reaches 1.2 MPa, and then the biogas is continuously introduced at the same flow rate, and at the same time
  • the absorbent regenerated in Example 6 was sent to the absorption tower 5 at a flow rate of 100 kg/h, and was sprayed into the tower from a nozzle in the upper portion of the column. In the process, the pressure inside the column was maintained at 1.2 MPa, and the temperature was 20 to 25 ° C.
  • the biogas is sufficiently contacted with the absorbent to remove carbon dioxide in the biogas, and the carbon dioxide-removing gas is dried to obtain a biomethane product gas, and the biomethane product gas is subjected to component analysis, and the methane content is 95.6%, the carbon dioxide is 3.7%, and the hydrogen sulfide is 34 ppm.

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  • Engineering & Computer Science (AREA)
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Abstract

L'invention concerne un procédé de préparation de biométhane par purification de biogaz. Le procédé comprend : la mise sous pression du biogaz, l'introduction du biogaz sous pression dans une tour d'absorption à partir de la partie inférieure de la tour d'absorption jusqu'à ce que la pression dans la tour atteigne 0,3 MPa à 20 MPa, l'introduction continue du biogaz, la pulvérisation d'un absorbant dans la tour au moyen d'une buse sur la partie supérieure de la tour d'absorption, et le fait de permettre au biogaz et à l'absorbant d'être suffisamment en contact pour éliminer le dioxyde de carbone dans le biogaz, la pression dans la tour d'absorption allant de 0,3 MPa à 20 MPa, et le rapport de débit de l'absorbant par rapport au biogaz étant de 8 à 100 kg/h:1 Nm3/h; l'absorbant est une solution aqueuse qui comporte au moins l'un parmi des solvants eutectiques à base de choline ou de liquides ioniques d'imidazole en tant qu'ingrédient actif, et la fraction massique de l'ingrédient actif va de 5 % à 90 %.
PCT/CN2014/094784 2014-11-28 2014-12-24 Procédé de préparation de biométhane par purification de biogaz WO2016082269A1 (fr)

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CN201410715418.0A CN104437008A (zh) 2014-11-28 2014-11-28 一种净化提纯沼气制备生物甲烷的方法
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