CN103304479B - Promoter for CO2 hydrate and application of promoter - Google Patents

Promoter for CO2 hydrate and application of promoter Download PDF

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Publication number
CN103304479B
CN103304479B CN201310204977.0A CN201310204977A CN103304479B CN 103304479 B CN103304479 B CN 103304479B CN 201310204977 A CN201310204977 A CN 201310204977A CN 103304479 B CN103304479 B CN 103304479B
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hydrate
temperature
pressure
promoter
gas
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CN103304479A (en
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李工
徐小军
张琳
王树立
周诗岽
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CHANGZHOU XIAOGUO INFORMATION SERVICES Co.,Ltd.
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Changzhou University
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Abstract

The invention relates to a promoter for generating a CO2 hydrate. The promoter is a low-concentration solution obtained by dissolving surface-active ion liquid into water, and the application concentration is 100-900 ppm; the surface-active ion liquid is respectively composed of 1-(3-sulfonic group) propyl hexamethyleneimine cations and dodecylbenzene sulfonic acid radical anions or 1-(3-sulfonic group) propyl pyrrolidine cations and the dodecylbenzene sulfonic acid radical anions. The promoter disclosed by the invention has a specific anion-cation structure and can be used for promoting the nucleation, growth and agglomeration of the CO2 hydrate, effectively lowering the phase equilibria point of the CO2 hydrate and shortening the generation induction time. Compared with the common promoter, the promoter disclosed by the invention has the advantages of more obvious promotion action, recycling capability, no pollution in a separation process, economy, environmental friendliness and high efficiency.

Description

A kind of CO2 hydrate accelerant and application thereof
Technical field
The invention belongs to chemical, environmental protection technical field, particularly relate to a kind of CO 2storage technology.
Background technology
Gas hydrate is a kind of nonstoichiometry cage compound being similar to ice that micro-molecular gas and water generate under cryogenic high pressure.In gas hydrate, form lattice structure between water molecules by stronger hydrogen bonded, gas molecule utilizes the Van der Waals force between water molecules to be filled in interlattice cage, and does not have stoichiometric relation between gas and water.In numerous gas hydrate species, due to CO 2the special property of gas and effect, CO 2hydrate receives the fervent concern in the whole world.
The world today, CO 2gas discharges in a large number and causes global warming, and environmental problem has become whole world important topic urgently to be resolved hurrily.The country of China's to be one with coal be main energy sources, wherein most coal is mainly used in thermal power generation, CO in power generation process 2quantity discharged is very large, causes China CO 2discharge situation very severe, suffered environment and international pressure increasing.Present stage, CO 2controlling mainly to comprise three aspects: reclaim separation, store transport, trans-utilization, wherein reclaim isolation technique energy consumption, cost is the highest, is restriction CO 2the key factor of emission control is also CO 2the first step recycled.
Reclaim and be separated containing CO 2the main method of gaseous mixture has physical absorption, chemical absorption, pressure-variable adsorption and membrane sepn etc.Waste gas is introduced absorption liquid purification by physical absorption, after liquid to be absorbed is saturated through heating, resolve, condensation reclaims, be applicable to the waste gas of atm number, low temperature, lower concentration, but need be equipped with and add Thermal desorption retrieving arrangement, equipment volume is large, investment is higher.Chemical absorption range of application is narrow, and it is large that absorption agent reclaims energy consumption.The subject matter that pressure swing adsorption process exists is that energy consumption is high, facility investment large, absorption utilization ratio is low.And now widely used membrane sepn rule has chemistry and poor heat stability, selectivity and flux are not high, processing power is limited, product purity is low etc. shortcoming.In the last few years, hydrate reclaimed, was separated, sealed CO up for safekeeping 2technology is subject to the extensive concern of international scholar.Hydrate is utilized to reclaim separation of C O 2technology has the following advantages:
(1) gas storage density is large.In normal conditions, 1m 3hydrate can store 150m 3above gas.
(2) CO is generated 2hydrate condition comparatively easily realizes.CO 2hydrate just can generate under pressure 1 ~ 5Mpa, temperature 0 DEG C ~ 10 DEG C conditions.
(3) storage security.CO 2the thermophysical property of hydrate is more stable, at 10 DEG C, under condition of normal pressure, and CO 2hydrate discharges gas completely needs more than 2 hours, than liquid CO 2storage method safety a lot.
(4) can absorb or release a large amount of heat when gas hydrate decomposes or generates.Therefore can be used as the cold storage agent in Cool Storage Technology, be than with the more effective a kind of Cool Storage Technology of other medium cold-storages.
(5) Application Areas is extensive.CO 2hydrate can be used for food fresh keeping, sea water desaltination, gas delivery, solution concentrate, the fields such as sewage disposal.
CO 2the generation of hydrate is a crystallisation process slowly, and along with gas-solid-liquid three-phase mass-and heat-transfer process, induction time is long, the speed of growth is slow, the hydrate generated at first can be gathered in liquid-gas interface, stops gas to enter liquid phase, hinders the further generation of hydrate.
Chinese patent CN102603674A discloses class gas hydrate accelerant [HMIPS] OTs and [HMIPS] Ss, proposes to utilize ionic liquid N +with strong positive charge, strengthen the hydrogen bond action in water, reduce CO 2balancing each other a little of hydrate.But because [HMIPS] Ss and [HMIPS] Ots is under the concentration of 100ppm ~ 900ppm, it is measure by the full-automatic surface tension instrument of QBZY_1 type that Shanghai Fang Rui Instrument Ltd. produces that surface tension reaches 73.3 ~ 74.8mN/m(surface tension), cause CO 2it is more difficult that gas enters into liquid phase, fails to solve the long problem of induction time.
Summary of the invention
Technical problem to be solved by this invention is: in prior art, the generation of carbon dioxide hydrate, there is the problem that induction time is long.
For solving this technical problem, the technical solution used in the present invention is: the invention provides a kind of CO 2hydrate accelerant, this CO 2hydrate accelerant is a kind of surface-active ion liquid, and wherein, the positively charged ion of ionic liquid is selected from, 1-(3-sulfonic group) cyclohexyl iminium cations or 1-(3-sulfonic group) propyl pyrrole alkane positively charged ion; Negatively charged ion is Witco 1298 Soft Acid root negatively charged ion.This surface-active ion liquid accelerator has following chemical structure:
In ionic liquid, the N in nitrogenous organic cyclic cationic +the intensity of hydrogen bond in water can be strengthened, reduce CO 2hydrate balance each other a little, its ring be conducive to hydrate nucleus generate;
There is surface-active negatively charged ion, effectively can reduce the surface tension of the aqueous solution, and there is the effect of foaming, solubilising, and with ionic liquid, nitrogenous organic cyclic cationic forms synergistic effect, shortens induction time.
Above-mentioned CO 2hydrate accelerant, when embody rule, is operating as: first surface-active ion liquid-mixing is made the certain density aqueous solution, and concentration range is 100ppm ~ 900ppm,
(1) in autoclave, inject the aqueous solution of above-mentioned surface-active ion liquid, open pumped vacuum systems, extract the gas in reactor and pipeline, pumpdown time 30min;
(2) control bath temperature, keep temperature in the kettle to stablize, in reactor, pass into CO with topping-up pump and air compressor machine 2gas, stops air inlet after reaching specified pressure, when reaction under high pressure temperature in the kettle drops to design temperature, opens magnetic stirring apparatus in still, and starts timing, at this moment, and CO 2hydrate generates fast, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is CO 2the induction time of hydrate,
Wherein, temperature in the kettle is 2 DEG C ~ 10 DEG C, and specified pressure is 3 ~ 5Mpa, and when the magnetic stirring apparatus in still works, rotating speed is 500 revs/min;
(3) after temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, opens vent valve, controls exhaust velocity (5 ~ 7 second pressure drop 0.01Mpa), keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, by sight glass visor, finds CO 2hydrate balance each other a little,
After opening vent valve, hydrate starts to decompose, and when there is obvious speck in glass visor, records equilibrium now, i.e. CO 2balancing each other a little of hydrate.
The invention has the beneficial effects as follows: the present invention will have surface-active ionic liquid first and be used for CO 2hydrate formation promoter, under zwitterion synergy, is conducive to CO 2gas enters liquid phase, promotes CO 2the nucleation of hydrate, growth, agglomeration, effectively reduce CO 2hydrate induction time, reduces CO 2hydrate balance each other a little, the effect of its promotor is better than simple ionic liquid and simple tensio-active agent.Surface-active ion liquid accelerator of the present invention is at CO 2hydrate discharges CO after heating up and reducing pressure 2after can reuse, environmental protection, efficient.Can be applied in fields such as hydrate storage and transportation gas technology, hydrate separation technology.
Accompanying drawing explanation
Fig. 1 is 1-(3-sulfonic group) cyclohexyl imines Witco 1298 Soft Acid, different concns dilute solution surface tension at different temperatures.
Fig. 2 is 1-(3-sulfonic group) propyl pyrrole alkane Witco 1298 Soft Acid, different concns dilute solution surface tension at different temperatures.
As can be seen from accompanying drawing: hydrate accelerant solution of the present invention, when concentration is 100ppm ~ 900ppm, surface tension is 32.8 ~ 48.5mN/m, compare the surface tension 73.3 ~ 74.8mN/m of [HMIPS] Ss and [HMIPS] OTs solution, fall is 55.8% to the maximum, can promote CO 2gas enters into liquid phase.
Above surface tension is all that the full-automatic surface tension instrument of QBZY_1 type using Shanghai Fang Rui Instrument Ltd. to produce measures.
Embodiment
Embodiment 1
In autoclave, inject 100ppm1-(3-sulfonic group) the cyclohexyl imines dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 2.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 70s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 2.0 DEG C, 1.51Mpa.
Embodiment 2
In autoclave, inject 300ppm1-(3-sulfonic group) the cyclohexyl imines dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 4.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.50Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 110s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 4.0 DEG C, 1.87Mpa.
Embodiment 3
In autoclave, inject 700ppm1-(3-sulfonic group) the cyclohexyl imines dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 6.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 4.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 200s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 6.0 DEG C, 2.42Mpa.
Embodiment 4
In autoclave, inject 900ppm1-(3-sulfonic group) the cyclohexyl imines dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 10.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 5.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 500s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 10.0 DEG C, 4.27Mpa.
Embodiment 5
In autoclave, inject 100ppm1-(3-sulfonic group) the propyl pyrrole alkane dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 2.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 60s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 2.0 DEG C, 1.46Mpa.
Embodiment 6
In autoclave, inject 300ppm1-(3-sulfonic group) the propyl pyrrole alkane dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 4.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.50Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 95s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 4.0 DEG C, 1.82Mpa.
Embodiment 7
In autoclave, inject 500ppm1-(3-sulfonic group) the propyl pyrrole alkane dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 8.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 4.50Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 300s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 8.0 DEG C, 3.02Mpa.
Embodiment 8
In autoclave, inject 700ppm1-(3-sulfonic group) the propyl pyrrole alkane dodecylbenzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 6.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 4.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 180s, i.e. CO 2hydrate induction time.
After temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, now, opens vent valve, controls exhaust velocity (5 ~ 7 seconds pressure drop 0.01Mpa), decomposition of hydrate, keeps temperature in the kettle constant, by pressure transmitter, temperature, pressure data is transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, when there is obvious speck in glass visor, records equilibrium now, now CO 2hydrate phase balance data are 6.0 DEG C, 2.44Mpa.
Comparative example 1
Other experiment conditions are identical with embodiment 3, only change the kind of hydrate accelerant:
In autoclave, inject 700ppm1-(3-sulfonic group) cyclohexyl imines hydrosulfate ([HMIPS] Ss) solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 6.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 4.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 550s, i.e. CO 2hydrate induction time.
Comparative example 2
Other experiment conditions are identical with embodiment 3, only change the kind of hydrate accelerant:
In autoclave, inject the 700ppm Sodium dodecylbenzene sulfonate solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 6.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 4.00Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 450s, i.e. CO 2hydrate induction time.
6 DEG C time, under original pressure 4.0MPa condition, the induction time 610s of pure aquatic system, as can be seen from comparative example 1,2, employ other hydrate accelerant, the limited extent that induction time declines, and use surface-active ion liquid of the present invention as hydrate accelerant, the amplitude that induction time declines is fairly obvious.
Comparative example 3
Other experiment conditions are identical with embodiment 6, only change the kind of hydrate accelerant:
In autoclave, inject 300ppm1-(3-sulfonic group) the cyclohexyl imines p-methyl benzenesulfonic acid solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 4.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.50Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 510s, i.e. CO 2hydrate induction time.
Comparative example 4
Other experiment conditions are identical with embodiment 6, only change the kind of hydrate accelerant:
In autoclave, inject the 300ppm Sodium dodecylbenzene sulfonate solution of 200mL, vacuumize 30min.
Open water bath with thermostatic control, controlling bath temperature is 4.0 DEG C, passes into the CO of 99.9% in reactor 2gas, stops air inlet after reaching 3.50Mpa, opens magnetic stirring apparatus (500 revs/min) in still, and starts timing, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is 400s, i.e. CO 2hydrate induction time.
4 DEG C time, under original pressure 3.50MPa condition, the induction time 550s of pure aquatic system, as can be seen from comparative example 3,4, employ other hydrate accelerant, the limited extent that induction time declines, and use surface-active ion liquid of the present invention as hydrate accelerant, the amplitude that induction time declines is fairly obvious.

Claims (1)

1. a CO 2the application of hydrate accelerant, is characterized in that: described application is specially, and first surface-active ion liquid-mixing is made the certain density aqueous solution, and concentration range is 100ppm ~ 900ppm,
Wherein, the positively charged ion of surface-active ion liquid is 1-(3-sulfonic group) cyclohexyl iminium cations or 1-(3-sulfonic group) propyl pyrrole alkane positively charged ion; Negatively charged ion is Witco 1298 Soft Acid root negatively charged ion,
(1) in autoclave, inject the aqueous solution of above-mentioned surface-active ion liquid, open pumped vacuum systems, extract the gas in reactor and pipeline, pumpdown time 30min;
(2) control bath temperature, keep temperature in the kettle to be stabilized in 2 DEG C ~ 10 DEG C, in reactor, pass into CO with topping-up pump and air compressor machine 2gas, stops air inlet after reaching specified pressure 3-5MPa, when reaction under high pressure temperature in the kettle drops to design temperature, opens magnetic stirring apparatus in still, and starts timing, at this moment, and CO 2hydrate generates fast, when having visible CO in glass visor 2when hydrate nucleus occurs, required time is CO 2the induction time of hydrate;
(3) after temperature, pressure remains unchanged in autoclave, CO can be thought 2hydrate generates completely, opens vent valve, control exhaust velocity, 5 ~ 7 second pressure drop 0.01MPa, keep temperature in the kettle constant, by pressure transmitter, temperature, pressure data are transferred to computer, record CO 2the temperature, pressure of hydrate in decomposition course, by sight glass visor, when occurring obvious speck in glass visor, records equilibrium now, i.e. CO 2balancing each other a little of hydrate.
CN201310204977.0A 2013-05-28 2013-05-28 Promoter for CO2 hydrate and application of promoter Active CN103304479B (en)

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