CN104403711A - Method and apparatus for separating CO2 in biogas based on hydrate process - Google Patents
Method and apparatus for separating CO2 in biogas based on hydrate process Download PDFInfo
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Abstract
The invention discloses a method and an apparatus for separating CO2 in biogas based on a hydrate process. The apparatus comprises a gas booster pump, a gas cooler, a hydrate reaction kettle, a hydrate slurry heater, a liquid booster pump, a liquid cooler, a gas chromatograph, a data acquisition and processing unit, valves and a pipeline; the hydrate reaction kettle is inside plated with a titanium layer for preventing more and more hydrate from being aggregated on the wall of the reaction kettle and solving the problems that a hydrate slurry in a hydrate separation gas is aggregated in the reaction kettle and circulation is not smooth; and the hydrate reaction kettle employs an outer jacket cooling and inner coil pipe cooling method, and also is coated with a thermal-insulation material layer at the outside, so that a large cooling environment in the hydrate reaction process is guaranteed, heat loss is reduced, and also the temperature in the hydrate reaction kettle is uniform. The apparatus structure is simple, the technology is relatively simple, more energy is saved, and the separation effect on biogas is relatively good.
Description
Technical field:
The present invention relates to mixed gas separation technology field, be specifically related to a kind of based on CO in hydrate separation biogas
2method and device.
Background technology:
Biogas be organic substance under anaerobic, a kind of mixed gas of generating through the fermentative action of microorganism, general containing methane 50 ~ 70%, all the other are carbonic acid gas and a small amount of nitrogen, hydrogen and hydrogen sulfide etc.Its characteristic is similar to Sweet natural gas, is a kind of new forms of energy having application prospect, and its exploitation are effective behaves of rural energy supply problem under solution energy shortage situation, and therefore, its development is subject to the attention of country day by day
CO in biogas
2, H
2the sour gas such as S usually have adverse influence in biogas utilization, therefore need to remove.The method removing foreign gas in biogas conventional at present mainly contains compression separation of liquid CO
2method, membrane separation process etc.But the method observable index that compression is separated is higher, and membrane separating method technics comparing is complicated, simultaneously to CH
4consumption also larger.
Gas hydrate gas separation is a kind of approach of effective separation different sorts gas.It utilizes the phase balance condition of gas with various guest molecule formation required for hydrate and the difference of complexity, make certain gas molecule and water water generation reaction compound, and nonreactive gas stays in the gas phase, to reach the effect of gas delivery.The method device is simple, and reaction conditions is gentle, easy to operate, CO
2uptake rate is high, and after being separated, biogas purity is high, and the aqueous solution can recirculation utilize, more friendly to environment.
Summary of the invention:
The object of this invention is to provide a kind of based on CO in hydrate separation biogas
2method and device.
The present invention is achieved by the following technical programs:
A kind of based on CO in hydrate separation biogas
2device, include the gas boosting pump for biogas being pressurized to predetermined pressure, the gas cooler being cooled to preset temperature, hydrate reaction still, hydrate slurry well heater, liquid booster pump, liquid cooler, gas chromatograph, data gathering and processing unit and valve and pipeline;
Described hydrate reaction still wall adopts jacket structured, and be followed successively by refrigeration agent interlayer, adiabator layer from inside to outside, described refrigeration agent interlayer internal recycle has refrigeration agent, and temperature adopts outside water bath with thermostatic control to control setting; Described hydrate reaction still kettle inside is coated with titanium layer, is provided with refrigerating coil in reactor; Described hydrate reaction still kettle top Flange joint has kettle cover, and described kettle cover is provided with evacuate air and collects the pressure transmitter of gaseous pressure in valve, monitoring hydrate reaction still and detect the temperature sensor of gas phase temperature and liquidus temperature in hydrate reaction still respectively; Described hydrate reaction still upper end is provided with solution spraying device; The hydrate slurry outlet that described hydrate reaction still lower end is provided with mechanical stirring device, gas feed, vacuum-pumping valve and follows hydrate slurry well heater to be communicated with; One-way cock has been installed in described gas feed place;
The temperature sensor that described data gathering and processing unit comprise data collecting instrument, connect with described data acquisition process instrument and pressure transmitter; Described temperature sensor is respectively used to monitor described gas cooler, hydrate reaction still liquid phase, hydrate slurry well heater, the temperature of liquid cooler, described pressure transmitter for monitoring described hydrate reaction still pressure;
Described gas boosting pump is communicated with the gas feed of hydrate reaction still via gas cooler; The collection and confinement of gases valve that described hydrate reaction still kettle cover is provided with is connected with gas flow dryer and gas chromatograph; The fluid inlet that hydrate slurry outlet is connected with hydrate slurry well heater, liquid booster pump and liquid cooler in turn, hydrate reaction still upper end is provided with that described hydrate reaction still lower end is provided with, forms a loop.
Described hydrate reaction still is made up of high voltage bearing stainless steel, and described refrigeration agent interlayer internal recycle has refrigeration agent, lowers the temperature to material in hydrate reaction still still or heats up, and cooling and temperature-rise period and refrigeration temperature adopt exterior terminal to control to set.
The adiabator layer of described hydrate reaction still wall, makes heat loss reach minimum as far as possible.Refrigerating coil is provided with, to increase the refrigerating duty in hydrate reaction process in described hydrate reaction still.
Described kettle inside is coated with titanium layer to increase wall hydrophobicity, avoids hydrate slurry to generate at reactor wall.
Described solution spraying device, evenly sprays the aqueous solution in hydrate reaction still, increases the contact area of solution and gas.
Described hydrate reaction still side is provided with form, can monitor the whole process of hydrate reaction.
Described hydrate slurry well heater is used for thermal degradation from the hydrate slurry bottom described hydrate reaction still, the CO after decomposition
2gas is discharged by valve, collect after be used as industrial raw material, the remaining aqueous solution then by be delivered in liquid cooler after liquid booster pump supercharging be cooled to reactor set temperature after enter hydrate reaction still.
Described gas cooler, hydrate reaction still, hydrate slurry well heater and liquid cooler are respectively by water bath with thermostatic control control temperature.
The present invention also provides a kind of and is separated CO in biogas based on hydrate
2method, utilize said apparatus, comprise the following steps:
A, raw material biogas is pressurized to 2-5MPa by gas boosting pump, and pass into gas cooling chamber and be cooled to 273-280K, then gas is passed in the hydrate reaction still after vacuumizing, ensure that gas does not reflux by unidirectional stop valve, temperature in the kettle controls between 273-280K by water bath with thermostatic control, and pressure-controlling is between 2-5MPa; Simultaneously, mass concentration needed for being generated by hydrate is evenly being sprayed in reactor gas phase by spray equipment containing the promotor aqueous solution of 0-40%, open reactor lower mechanical whipping appts, impel the aqueous solution and gas fully to contact generation hydrate reaction, the total amount of described spray solution reaches the volume of reactor 3/4;
B, after hydrate reaction terminates, discharge generate hydrate slurry, and by hydrate slurry heater heats decompose generate hydrate, CO hydrate collected by valve
2discharge Deng sour gas, reclaim again to be sent in hydrate reaction still after the aqueous solution obtained to be sent in liquid cooler cooling after liquid booster pump supercharging simultaneously and reuse; In hydrate reaction still, residual gas is after super-dry, uses chromatographic gaseous fraction, if meet with gas requirement, directly exports, if do not meet, circulation passes into the reaction of hydrate reaction still until meet the requirements again.
The total amount of described spray solution reaches the volume of reactor 3/4, the density of hydrate slurry is declined, is beneficial to CO most
2the separation of gas, and be beneficial to transporting of hydrate slurry most, avoids hydrate to lump in reactor gathering.
Beneficial effect of the present invention is as follows:
1, the inner titanizing layer of described hydrate reaction still, avoids hydrate to be more and more gathered on reactor wall, solves hydrate slurry in hydrate separation gas in the past and assemble in a kettle. thus the not smooth problem that circulates;
2, hydrate reaction still of the present invention adopts external jacket refrigeration and the cold dual refrigeration method of inner disk control, the coated adiabator layer in outside simultaneously, wherein external jacket and inner coil pipe freeze respectively, refrigerating environment large in hydrate reaction process can be ensured, reduce heat loss, hydrate reaction temperature in the kettle can be made again even.
3, be provided with mechanical stirring device bottom hydrate reaction still, reactor top is provided with solution spraying device, will stir and combine with spray, and increase the contact area of high pressure gas and the aqueous solution as much as possible, and promote the generation of hydrate.
4, the aqueous solution containing promotor needed for hydrate generation reacts with water to generate the guest molecule of half Study of Clathrate Hydrates and the mixed aqueous solution of tensio-active agent, this mixing solutions effectively can reduce the temperature and pressure condition required for hydrate generation, being separated of the generation of hydrate and gas can also be promoted, again large harm is not caused to environment, not corrosion reacting kettle.
5, the hydrate slurry generated after hydrate reaction discharges reactor by valve, then makes it be separated into gas and the aqueous solution through heating, and reclaims respectively, and gas can be used as industrial raw material, and the aqueous solution can repeat recycling.
6, hydrate reaction still pneumatic outlet connects gas chromatograph, monitors CH in gas reactor at any time
4, CO
2and H
2the content of S, as long as gaseous fraction reaches the standard with gas, can export gas at any time.
In a word, the application's structure is simple, and technique is simpler, more energy-conservation, for biogas (CO
2comparision contents is high) separating effect better.
Accompanying drawing illustrates:
Fig. 1 is structural representation of the present invention;
Fig. 2 is the sectional view of hydrate reaction still;
Wherein, 1. gas boosting pump, 2. tensimeter, 3. temperature sensor, 4. water bath with thermostatic control, 5. gas cooler, 6. unidirectional stop valve, 7. pressure transmitter, 8. temperature sensor, 9. temperature sensor, 10. data collecting instrument, 11. hydrate reaction stills, 12. forms, 13. vacuum pump 14. liquid-inlet pipes, 15. waters bath with thermostatic control, 16. hydrate slurry well heaters, 17. waters bath with thermostatic control, 18. temperature sensors, 19. liquid booster pumps, 20. liquid coolers, 21. temperature sensors, 22. gas flow dryers, 23. gas chromatographs, 24. refrigeration agents are imported and exported, 25. adiabator layers, 26. refrigerating coils are imported and exported, 27. reactor supports, 28. mechanical stirring devices, 29. refrigerating coils, 30. refrigeration agent interlayers, 31. solution spraying devices, 32. joint flanges, V1-V10. valve.
Embodiment:
Below further illustrate of the present invention, instead of limitation of the present invention.
A kind of based on CO in hydrate separation biogas
2device, as shown in Figure 1, the gas boosting pump 1 for biogas being pressurized to predetermined pressure, the gas cooler 5 being cooled to preset temperature, hydrate reaction still 11, hydrate slurry well heater 16, liquid booster pump 19, liquid cooler 20, gas chromatograph 23, data gathering and processing unit and valve V1-V10 and pipeline is included;
As shown in Figure 2, described hydrate reaction still 11 wall adopts jacket structured, and be followed successively by refrigeration agent interlayer 30, adiabator layer 25 from inside to outside, described refrigeration agent interlayer 30 internal recycle has refrigeration agent, and refrigeration temperature adopts outside water bath with thermostatic control 15 to control setting; Described hydrate reaction still 11 kettle inside is coated with titanium layer, is provided with refrigerating coil 29 in reactor; There is kettle cover on described hydrate reaction still 11 kettle top by joint flange 32 Flange joint, and described kettle cover is provided with evacuate air and collects the pressure transmitter 7 of gaseous pressure in valve V7, monitoring hydrate reaction still 11 and detect the temperature sensor 8,9 of gas phase temperature and liquidus temperature in hydrate reaction still 11 respectively; Described hydrate reaction still 11 upper end is provided with solution spraying device 31; The hydrate slurry outlet that described hydrate reaction still 11 lower end is provided with mechanical stirring device 28, gas feed, vacuum-pumping valve and follows hydrate slurry well heater 16 to be communicated with; One-way cock 6 has been installed in described gas feed place;
The temperature sensor 3,8,9,18,21 that described data gathering and processing unit comprise data collecting instrument 10, connect with described data acquisition process instrument 10 and pressure transmitter 7; Described temperature sensor 3,8,9,18,21 is respectively used to the temperature of monitoring described gas cooler 5, hydrate reaction still 11 liquid phase, hydrate slurry well heater 16, liquid cooler 20;
Described gas boosting pump 1 is communicated with hydrate reaction still 11 gas feed via gas cooler 5; The collection and confinement of gases valve that described hydrate reaction still 11 kettle cover is provided with is connected with gas flow dryer 22 and gas chromatograph 23; The fluid inlet that hydrate slurry outlet is connected with hydrate slurry well heater 16, liquid booster pump 19 and liquid cooler 20 in turn, hydrate reaction still 11 upper end is provided with that described hydrate reaction still 11 lower end is provided with, forms a loop.
Said apparatus is utilized to be separated CO in biogas based on hydrate
2method as follows:
1. open valve V1, unstripped gas is passed in topping-up pump 1 and be pressurized to certain pressure (according to CH in raw material biogas
4content different, pressure range is between 2-5MPa), pressure value is read by tensimeter 2.Then Open valve V2, passed in gas cooler 5 by the unstripped gas after supercharging and be cooled to 273-280K, gas cooler 5 is lowered the temperature by water bath with thermostatic control 4, and temperature is controlled by temperature sensor 3.
2. open valve V3, vacuum pump 13 is utilized to be vacuumized by hydrate reaction still, cooled high pressure feed is passed in hydrate reaction still 11 through unidirectional stop valve 6, refrigerating coil 26 in water bath with thermostatic control 15 and reactor is utilized temperature of reaction kettle to be reduced to suitable temp (temperature range is between 273-280K), in reaction process, reacting kettle inner pressure numerical value is gathered by pressure transmitter 7, gas phase temperature and liquidus temperature are gathered by temperature sensor 8 and 9 respectively, gather numerical value and are collected by data collecting instrument 10.
3. after temperature of reaction kettle is reduced to design temperature, open reactor solution spraying device 31 and mechanical stirring device 28, make the aqueous solution and the abundant contact reacts of high pressure feed generate hydrate.
4., after hydrate reaction terminates, when namely pressure transmitter numerical value 7 no longer changes, open valve V4, the hydrate slurry of generation is transported in solution heater 16 and heats, solution heater temperature is controlled by water bath with thermostatic control 17, is set in 300K, fully to decompose hydrate slurry.CO after decomposition
2gas is discharged by valve V5, collects, and can be used as industrial raw material further.The remaining aqueous solution continues through valve V6 after being delivered to after then carrying out supercharging by liquid booster pump 19 and being cooled to reactor set temperature in liquid cooler 20 and liquid-inlet pipe 14 enters participation reaction in hydrate reaction still.
5. open valve V8, the purifying gas in reactor is carried out drying through moisture eliminator 22, then utilize gas chromatograph 23 pairs of gases to carry out composition analysis, work as CH
4when component concentration reaches requirement, open valve V9, gas is exported by 3-way valve V10, when foreign gas content does not reach standard, then gas is circulated again.
Embodiment 1
Get unstripped gas sample, wherein CH
4content is 60%, CO
2content is 40%, and choose the SDS aqueous solution that mass concentration is 300ppm, temperature of reaction kettle is 278K, when pressure is 5MPa, after reaction 30min, and CH in reactor gas phase
4content bring up to 90.8%, CO
2content be 9.2%, then through once circulation after, CH in reactor gas phase
4content be 97.1%, CO
2content be 2.9%.
Embodiment 2
Get unstripped gas sample, wherein CH
4content is 50%, CO
2content is 50%, and choose the TBAB aqueous solution that mass concentration is 0.05%, temperature of reaction kettle is 276K, when pressure is 3.5MPa, after reaction 30min, and CH in reactor gas phase
4content be 88.8%, CO
2content be 11.2%, after decomposition of hydrate, unstripped gas again through 2 times circulation after, CH in reactor gas phase
4content be 95.3%, CO
2content be 4.7%.
Embodiment 3
Get unstripped gas sample, wherein CH
4content is 40%, CO
2content is 59%, H
2s content is 1%, and choose the SDS mixed aqueous solution that mass concentration is THF and 100ppm of 1%, temperature of reaction kettle is 278K, and pressure is 2.5MPa, after reaction 1h, and CH in gas phase in reactor
4content is 85.5%, CO
2content is 13.9%, H
2s content is 0.6%, after 3 circulations, and CH
4content is 95.2%, CO
2content is 4.2%, H
2s content is 0.4%.
Claims (3)
1. one kind is separated CO in biogas based on hydrate
2device, it is characterized in that, including the gas boosting pump (1) for biogas being pressurized to predetermined pressure, be cooled to the gas cooler (5) of preset temperature, hydrate reaction still (11), hydrate slurry well heater (16), liquid booster pump (19), liquid cooler (20), gas chromatograph (23), data gathering and processing unit and valve (V1-V10) and pipeline;
Described hydrate reaction still (11) wall adopts jacket structured, be followed successively by refrigeration agent interlayer (30), adiabator layer (25) from inside to outside, described refrigeration agent interlayer (30) internal recycle has refrigeration agent, and refrigeration temperature adopts outside water bath with thermostatic control (15) to control setting; Described hydrate reaction still (11) kettle inside is coated with titanium layer, is provided with refrigerating coil (29) in reactor; Described hydrate reaction still (11) kettle top Flange joint has kettle cover, and described kettle cover is provided with evacuate air and collection valve (V7), monitors the pressure transmitter (7) of hydrate reaction still (11) interior gaseous pressure and detect the temperature sensor (8,9) of hydrate reaction still (11) interior gas phase temperature and liquidus temperature respectively; Described hydrate reaction still (11) upper end is provided with solution spraying device (31); The hydrate slurry outlet that described hydrate reaction still (11) lower end is provided with mechanical stirring device (28), gas feed, vacuum-pumping valve and follows hydrate slurry well heater (16) to be communicated with; One-way cock (6) has been installed in described gas feed place;
The temperature sensor (3,8,9,18,21) that described data gathering and processing unit comprise data collecting instrument (10), connect with described data acquisition process instrument (10) and pressure transmitter (7); Described temperature sensor (3,8,9,18,21) is respectively used to the temperature of monitoring described gas cooler (5), hydrate reaction still (11) liquid phase, hydrate slurry well heater (16), liquid cooler (20);
Described gas boosting pump (1) is communicated with hydrate reaction still (11) gas feed via gas cooler (5); The collection and confinement of gases valve that described hydrate reaction still (11) kettle cover is provided with is connected with gas flow dryer (22) and gas chromatograph (23); The fluid inlet that hydrate slurry outlet is connected with hydrate slurry well heater (16), liquid booster pump (19) and liquid cooler (20) in turn, hydrate reaction still (11) upper end is provided with that described hydrate reaction still (11) lower end is provided with, forms a loop.
2. according to claim 1 based on CO in hydrate separation biogas
2device, it is characterized in that, described hydrate reaction still side is provided with form.
3. one kind is separated CO in biogas based on hydrate
2method, it is characterized in that, utilize device described in claim 1 or 2, comprise the following steps:
A, biogas is pressurized to 2-5MPa by gas boosting pump, and pass into gas cooling chamber and be cooled to 273-280K, then gas is passed in the hydrate reaction still after vacuumizing, ensure that gas does not reflux by unidirectional stop valve, temperature in the kettle controls between 273-280K by water bath with thermostatic control, and pressure-controlling is between 2-5MPa; Simultaneously, mass concentration needed for being generated by hydrate is evenly being sprayed in reactor gas phase by spray equipment containing the promotor aqueous solution of 0-40%, open reactor lower mechanical whipping appts, impel the aqueous solution and gas fully to contact generation hydrate reaction, the total amount of described spray solution reaches the volume of reactor 3/4;
B, after hydrate reaction terminates, discharge generate hydrate slurry, and by hydrate slurry heater heats decompose generate hydrate, CO hydrate collected by valve
2sour gas is discharged, and reclaims again to be sent in hydrate reaction still after the aqueous solution obtained to be sent in liquid cooler cooling after liquid booster pump supercharging to reuse simultaneously; In hydrate reaction still, residual gas is after super-dry, uses chromatographic gaseous fraction, if meet with gas requirement, directly exports, if do not meet, circulation passes into the reaction of hydrate reaction still until meet the requirements again.
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| CN110229043B (en) * | 2019-07-19 | 2022-08-30 | 深圳市燃气集团股份有限公司 | CH of hydrate method 4 /CO 2 Separation device and method |
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| CN111088087B (en) * | 2019-12-30 | 2021-07-20 | 广东瓦格耐电力科技有限公司 | Biogas pretreatment device for biogas generator set |
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