CN110152452A - A kind of non-aqueous solid-liquid phase change absorption system of ternary and its application - Google Patents

A kind of non-aqueous solid-liquid phase change absorption system of ternary and its application Download PDF

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CN110152452A
CN110152452A CN201910393822.3A CN201910393822A CN110152452A CN 110152452 A CN110152452 A CN 110152452A CN 201910393822 A CN201910393822 A CN 201910393822A CN 110152452 A CN110152452 A CN 110152452A
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solid
ternary
phase
liquid
phase change
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CN110152452B (en
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吕碧洪
荆国华
陈志标
周作明
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Huaqiao University
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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
    • B01D53/1456—Removing acid components
    • B01D53/1475—Removing carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/202—Alcohols or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/204—Amines
    • B01D2252/20436—Cyclic amines
    • B01D2252/20447—Cyclic amines containing a piperazine-ring
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention discloses a kind of non-aqueous solid-liquid phase change absorption system of ternary and its application, the triplex mixture system being made of 2-amino-2-methyl-1-propanol, dimethyl ether and piperazine, the system absorbs CO2Preceding is transparent and homogeneous liquid solution, absorbs CO2After become solid-liquid two-phase, and CO2It is enriched in solid phase, only needs to regenerate after separating solid phase, regenerated rich solution amount can be greatly reduced, to reduce the regeneration energy consumption of technology.The solid-liquid phase change ternary absorption system, maximum advantage is that the rich solution solid phase after saturation is granule crystal, compared with the existing thick rich solution of solid-liquid phase change system solid phase of tradition, easily separated operation；And the phase transformation system regeneration temperature is far below traditional solid-liquid phase change system, therefore has better application prospect.

Description

A kind of non-aqueous solid-liquid phase change absorption system of ternary and its application
Technical field
The invention belongs to collecting carbonic anhydride technical fields, and in particular to a kind of non-aqueous solid-liquid phase change absorption system of ternary And its application.
Background technique
Carbon dioxide (CO2) it is used as most important greenhouse gases, control and the hot spot that emission reduction is that various countries are paid close attention in recent years. Carbon emission reduction is primarily directed to energy resource system, such as thermal power plant CO2Emission source is concentrated, key is to CO in flue gas2Trapping Separation.But traditional organic amine aqueous solution absorption process has that regeneration energy consumption is high.By taking 30wt% ethanol amine (MEA) as an example, The thermal desorption energy consumption of its saturated solution is up to 3.7GJ/t CO2, a large amount of energy consumption is in the heating and evaporation process of aqueous solvent.
Phase transformation absorbent is as a kind of New Absorbent, in recent years by the extensive concern of researchers.This novel suction Agent is received, CO is being absorbed2Preceding is homogeneous phase solution, absorbs CO2It can make absorbent that liquid-liquid or solid-occur by the adjusting of certain means afterwards Liquid split-phase, CO2It mainly is enriched in a wherein phase, it only need to be by CO2Richness is mutually sent to desorbing in regenerator, so that absorbent be greatly decreased Regeneration volume, and then reduce the regeneration energy consumption of the system.Currently, being concentrated mainly on liquid-liquid phase in existing phase transformation absorbent Become absorption system, but in fact, the research of the system is still not yet mature, such as liquid-liquid two-phase laminated flow is inconvenient, rich solution viscosity compared with The problems such as big, still needs to by further studying and exploration is solved.In addition to liquid-liquid split-phase, the research and development energy of solid-liquid split-phase system Liquid-liquid split-phase system problem encountered is overcome to a certain extent.Due to CO2Absorption product is constantly in solid form from molten It is precipitated out in liquid, is conducive to the quick separating of product.The existing research about solid-liquid phase change absorbent is based on organic amine Based on the non-aqueous solid-liquid phase change system of polyamine, the solid product of formation is thick object, is unfavorable for separating；And base (polyamine) non-aqueous solid-liquid phase change system, can make CO2Absorption product is precipitated out completely from solvent, is had more preferable Split-phase effect, but excessively high regeneration temperature easily accelerates the oxidative degradation of amine and the corrosion of equipment.Therefore, how to construct novel Solid-liquid phase change absorbent is a crucial problem.
It can be seen from the above, phase transformation absorbent, because of CO2It mainly is enriched in a wherein phase, it only need to be by CO2Richness is mutually sent to regenerator Interior desorption so that the regeneration volume of absorbent be greatly decreased, thus has huge energy-saving potential.Wherein, solid-liquid phase change absorbs Agent with liquid liquid phase become absorbent compared with, product is relatively easily separated, be more advantageous to practical operation, but correlative study is less, how structure Building novel solid-liquid phase change system is still a problem.The present invention propose a kind of non-aqueous solid-liquid phase change absorption system of ternary and its Carbon Dioxide Application is trapped, the sticky defect for being difficult to separate or regeneration temperature is high of existing phase transformation absorbent rich solution will be overcome, be Collecting carbonic anhydride provides new thinking.
Summary of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of non-aqueous solid-liquid phase change suction of ternary Acceptor system and its application solve the problems such as collecting carbonic anhydride low efficiency in above-mentioned background technique, absorbent regeneration is difficult.
The technical solution adopted by the present invention to solve the technical problems is: providing a kind of non-aqueous solid-liquid phase change suction of ternary Acceptor system, the ternary being made of 2-amino-2-methyl-1-propanol (AMP), dimethyl ether (DME) and piperazine (PZ) are mixed Zoarium system, wherein the mol ratio of 2-amino-2-methyl-1-propanol and piperazine is 7:3-9:1, and the two total concentration is 1- 2mol/L, dimethyl ether are solvent.
Wherein, AMP (formula I) is used as main absorbent, because of its space steric effect, the excellent regenerability of guarantee system；Base CO is absorbed in the non-aqueous Solid-liquid demixing system of AMP2Afterwards, product is generated in the form of a small amount of solid, needs regenerated absorbent volume Amount is greatly decreased, and at a lower temperature can highly efficient regeneration, energy-saving potential is huge；
DME (Formula II) is used as split-phase reagent, it is ensured that absorbent absorbs CO2Afterwards easily occur solid-liquid phase change, because its higher boiling, Low-vapor pressure characteristic, solvent is not volatile when regeneration；
Pz (formula III) is used as CO2The deprotonation activator of absorbing reaction, nucleophilicity organic base deprotonation activator Pz's adds Add, system can be significantly improved to CO2Absorbent properties, can make up AMP absorb CO2In terms of absorption rate and absorption load not Foot.
In a preferred embodiment of the present invention, the triplex mixture system is for absorbing in pure carbon dioxide or mixed gas Volume ratio is the carbon dioxide of 5-20%.
In a preferred embodiment of the present invention, the carbon dioxide absorption temperature of the triplex mixture system is 30-60 DEG C, is inhaled Receipts load is 0.5-1.0mol CO2/ mol absorbent.
In a preferred embodiment of the present invention, the triplex mixture system has split-phase performance.Individual AMP or Pz is dissolved in The binary system of DME composition absorbs CO2The equal no phase separation ability in front and back, but the ternary system of AMP+PZ+DME composition absorbs CO2Before be Transparent and homogeneous liquid solution absorbs CO2After become solid-liquid two-phase.
In a preferred embodiment of the present invention, the triplex mixture system is absorbing CO2Preceding is homogeneous phase solution, absorbs CO2Afterwards Become solid-liquid two-phase, wherein solid phase is granule crystal, and CO2It is enriched in solid phase, only needs to regenerate i.e. after separating solid phase Can, regenerated rich solution amount can be greatly reduced, to reduce the regeneration energy consumption of technology.The rich solution volume Zhan of the solid-liquid two-phase is total The 20-50% of volume, required regenerated rich solution amount are reduced, and further effectively reduce regeneration energy consumption.
In a preferred embodiment of the present invention, the solid phase of the solid-liquid two-phase is regenerated by thermal desorption mode.
In a preferred embodiment of the present invention, regeneration temperature is 90-120 DEG C, reproduction time 50-100min, revival Rate is 40%-95%.
The present invention also provides a kind of non-aqueous solid-liquid phase change absorption system of above-mentioned ternary answering in trapping carbon dioxide With.
In a preferred embodiment of the present invention, using 2-amino-2-methyl-1-propanol as main absorbent, dipropylene glycol two Methyl ether is as split-phase reagent, piperazine as CO2The deprotonation activator of absorbing reaction, three form triplex mixture system, absorb Volume ratio is the carbon dioxide of 5-20% in pure carbon dioxide or mixed gas, and absorbing temperature is 30-60 DEG C, absorbs load and is 0.5-1.0mol CO2/ mol absorbent.
In a preferred embodiment of the present invention, CO will be absorbed2The solid phase become in the system of solid-liquid two-phase afterwards is separated by filtration Afterwards, it is regenerated by thermal desorption mode, regeneration temperature is 90-120 DEG C, reproduction time 50-100min, regeneration efficiency 40%- 95%.
The technical program compared with the background art, it has the following advantages:
1. this programme efficiently uses each component advantage, the effect of 1+1+1 > 3 is obtained, using AMP as main absorbent, because of it Space steric effect, the excellent regenerability of guarantee system；DME is as split-phase reagent, it is ensured that absorbent absorbs CO2Yi Fasheng afterwards Solid-liquid phase change, because of its higher boiling, low-vapor pressure characteristic, solvent is not volatile when regeneration；Pz is as CO2Absorbing reaction goes matter System CO can be substantially improved in sub- activator2Absorbent properties, CO2Trapping performance is 0.5-1.0mol CO2/ mol absorbent；
2. passing through CO2The characteristic of system phase transformation may be implemented in the regulation of load, simple and efficient；
3. the rich solution solid phase after saturation is granule crystal, with the existing thick rich solution of solid-liquid phase change system solid phase of tradition It compares, easily separated operation, and regeneration temperature is far below traditional solid-liquid phase change system, overcomes existing phase transformation absorbent rich solution sticky It is difficult to the defect separated or regeneration temperature is high.
Detailed description of the invention
CO is trapped when Fig. 1 is AMP and the mol ratio of Pz is 7:32The phase transformation effect picture of front and back, wherein before a- absorbs, b- After absorption, c- solid phase rich solution；
Fig. 2 is different proportion AMP-PZ-DME ternary solid-liquid phase change system CO2Absorbability comparison；
Fig. 3 is AMP-PZ-DME ternary solid-liquid phase change system regenerability under different regeneration temperatures.
Specific embodiment
Embodiment 1
The non-aqueous solid-liquid phase change absorption system of a kind of ternary of the present embodiment, using 2-amino-2-methyl-1-propanol as master Absorbent, dimethyl ether are as split-phase reagent, piperazine as CO2The deprotonation activator of absorbing reaction, three's composition Triplex mixture system, wherein the mol ratio of 2-amino-2-methyl-1-propanol and piperazine is 7:3-9:1, the two total concentration For 1-2mol/L, dimethyl ether is solvent.
The carbon dioxide for being 5-20% for absorbing volume ratio in pure carbon dioxide or mixed gas；The present embodiment uses two Ratio in carbonoxide and nitrogen mixed gas is 0~20%, and absorbing temperature is 30~60 DEG C.
The ternary system of AMP-PZ-DME composition absorbs CO2Preceding is transparent and homogeneous liquid solution, absorbs CO2After become it is solid- Liquid two-phase, and solid phase is granular crystals.CO will be absorbed2Become leading to after the solid phase in the system of solid-liquid two-phase is separated by filtration afterwards Desorption mode regeneration is overheated, regeneration temperature is 90-120 DEG C, reproduction time 50-100min, regeneration efficiency 40%-95%.
Comparative example 1~3
1mol/L, 1.5mol/L, 2mol/L AMP aqueous solution and DME solution is respectively adopted and prepares binary mixture conduct Comparative example.
One, CO is absorbed2Afterload, split-phase effect detection: at 40 DEG C, detection embodiment 1 and comparative example 1~3 absorb CO2 Performance and split-phase effect
Method: the AMP-PZ-DME ternary system and 1~3AMP of comparative example aqueous solution and DME of 30g embodiment 1 are prepared respectively The binary mixture of solution, is respectively poured into three-necked flask, under 40 DEG C of heat preservations, is placed on 150r/min on magnetic stirring apparatus and is stirred It mixes, is passed through 60mLmin-1CO2Start to absorb test until absorbent is saturated.By this experiment, it can get different absorbents System absorbs CO2Rate change with time situation.Absorption rate and time relationship are integrated, different time is can get and absorbs Agent absorbs CO2Load condition.
As a result: Fig. 1 illustrate AMP and Pz mol ratio be 7:3 when, AMP-PZ-DME ternary solid-liquid phase change system inhale Receive CO2The photo of front and back and solid phase rich solution.It can be seen from the figure that AMP-PZ-DME absorbs CO2Preceding is uniform liquid phase, absorbs CO2 Become solid-liquid two-phase, CO after saturation2It mainly is enriched in solid phase, is graininess white crystal.It is absorbed with existing solid-liquid phase change solid Mutually thick difference, the particulate matter solid phase are very easy to be isolated by filtration, the volume of particle of the total volume 47%.This is consolidated After phase transfer pyrolysis regeneration, become again after being mixed with lean solution homogeneous.
As shown in Fig. 2, the ternary phase variant system of difference mol ratio AMP and Pz composition absorbs CO2Ability have significantly Difference.It with the increase of Pz content, absorbs load and gradually rises, but liquid-rich solid volume also increases.When AMP and PZ ratio is When 7:3, the carbon dioxide enriched solid volume after crystal grain solid phase, split-phase only 47%, CO of the total volume2Content but accounts for The 94% of gross absorption.And the AMP aqueous solution of comparative example and the binary mixture of DME solution absorb CO2No phase separation ability afterwards, And the individual aqueous solution of AMP absorbs CO2Also no phase separation ability afterwards.
Two, 1 regenerability of embodiment detects
Since Industry Waste is large-minded, the recycling utilization of absorbent is vital link, affect technique at This.Absorbent regeneration method common are thermal desorption, film filtering, transformation method etc..The regeneration method used in this experimental example is heat Desorption investigates the power of regeneration of absorbent by the absorption load before and after comparison absorbent regeneration.
Method: AMP-PZ-DME ternary solid-liquid phase change system (1M, 7:3) solution of Example 1, according in experimental example 1 CO is absorbed at 40 DEG C2To saturation.Absorbent after saturation is warm under (90,100,110,120 DEG C) under different regeneration temperatures 60min is desorbed, the absorbent after regeneration repeats absorption experiment according to method in experimental example 1, investigates different regeneration temperatures to absorption The influence of performance.
As a result: as shown in figure 3, AMP-PZ-DME ternary solid-liquid phase change system (1M, 7:3) solution is equal at 90~120 DEG C Regeneration can be achieved, but as the temperature rises, regeneration efficiency increases, wherein solid is not fully converted between 90 DEG C to 110 DEG C Liquid；And desorbed 60 minutes at 120 DEG C, solid is then completely converted into liquid, and regeneration efficiency reaches as high as 92%.Tradition has The regeneration temperature of machine amine aqueous solution is generally 120 DEG C, and traditional phase transformation amine absorbent can not almost be regenerated in the case where nitrogen-free air-blowing is swept, It is only 70-80% that nitrogen, which purges lower regeneration efficiency,；And the solid phase regeneration temperature of existing polyamine solid-liquid phase change absorbent is generally high In 120 DEG C.Therefore AMP-PZ-DME ternary solid-liquid phase change system described in this patent, in addition to phase transformation absorbent regeneration energy It consumes outside low advantage, also effectively overcomes the defect that existing phase transformation amine regeneration is difficult, regeneration temperature is high.
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.

Claims (10)

1. a kind of non-aqueous solid-liquid phase change absorption system of ternary, it is characterised in that: for by 2-amino-2-methyl-1-propanol, dipropyl The triplex mixture system of glycol dimethyl ether and piperazine composition, the wherein mol ratio of 2-amino-2-methyl-1-propanol and piperazine For 7:3-9:1, the two total concentration is 1-2mol/L, and dimethyl ether is solvent.
2. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 1, it is characterised in that: the ternary is mixed The carbon dioxide that zoarium system is 5-20% for absorbing volume ratio in pure carbon dioxide or mixed gas.
3. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 2, it is characterised in that: the ternary is mixed The carbon dioxide absorption temperature of zoarium system is 30-60 DEG C, and absorption load is 0.5-1.0mol CO2/ mol absorbent.
4. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 1, it is characterised in that: the ternary is mixed Zoarium system has split-phase performance, is absorbing CO2Preceding is homogeneous phase solution, absorbs CO2After become solid-liquid two-phase, wherein solid phase be particle Crystal, and CO2It is enriched in solid phase.
5. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 4, it is characterised in that: the solid-liquid two The rich solution volume 20-50% of the total volume of phase.
6. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 4, it is characterised in that: the solid-liquid two The solid phase of phase is regenerated by thermal desorption mode.
7. the non-aqueous solid-liquid phase change absorption system of a kind of ternary according to claim 6, it is characterised in that: regeneration temperature is 90-120 DEG C, reproduction time 50-100min, regeneration efficiency 40%-95%.
8. the non-aqueous solid-liquid phase change absorption system of a kind of ternary as described in any one of claims 1 to 7 is in trapping carbon dioxide Application.
9. application according to claim 8, it is characterised in that: using 2-amino-2-methyl-1-propanol as main absorbent, Dimethyl ether is as split-phase reagent, piperazine as CO2The deprotonation activator of absorbing reaction, three form ternary mixing System absorbs the carbon dioxide that volume ratio in pure carbon dioxide or mixed gas is 5-20%, and absorbing temperature is 30-60 DEG C, is inhaled Receipts load is 0.5-1.0mol CO2/ mol absorbent.
10. application according to claim 8, it is characterised in that: CO will be absorbed2Become consolidating in the system of solid-liquid two-phase afterwards It after being mutually separated by filtration, is regenerated by thermal desorption mode, regeneration temperature is 90-120 DEG C, reproduction time 50-100min, revival Rate is 40%-95%.
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