CN104403711B - 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 is and in particular to a kind of be based on co in hydrate separation biogas2
Method and device.
Background technology:
Biogas be organic substance under anaerobic, a kind of mixed gas of generating through the fermentation of microorganism,
Typically contain methane 50～70%, remaining is carbon dioxide and a small amount of nitrogen, hydrogen and hydrogen sulfide etc..Its characteristic is similar to natural gas,
It is a kind of new forms of energy of great application prospect, it develops is to solve the having of rural energy supply problem under energy shortage situation
Effect behave, therefore, its development is increasingly subject to the attention of country
Co in biogas2, h2The sour gas such as s usually have detrimental effect it is therefore desirable to remove in biogas utilization.Mesh
The method removing foreign gas in front conventional biogas mainly has compression to separate liquid co2Method, membrane separation process etc..But, compression
Detached method observable index is higher, and membrane separating method technics comparing is complicated, simultaneously to ch4Consumption also than larger.
Gas hydrates gas separation is a kind of approach efficiently separating variety classes gas.It is using different
Phase balance condition required for gas guest molecule formation hydrate and the difference of complexity, make certain gas molecule and water
Reaction generates hydrate, and nonreactive gas stays in the gas phase, to reach the detached effect of gas.Party's subtraction unit is simple,
Reaction condition is gentle, easy to operate, co2Absorption rate is high, and after separating, biogas purity is high, and the aqueous solution being capable of repetitive cycling profit
With more friendly to environment.
Content of the invention:
It is an object of the invention to provide a kind of be based on co in hydrate separation biogas2Method and device.
The present invention is achieved by the following technical programs:
One kind is based on co in hydrate separation biogas2Device, include for biogas is pressurized to predetermined pressure
Gas boosting pump, the gas cooler being cooled to predetermined temperature, hydrate reaction kettle, hydrate slurry heater, liquid supercharging
Pump, liquid chiller, gas chromatograph, data acquisition and processing unit and valve and pipeline；
Described hydrate reaction kettle wall, using jacket structured, is followed successively by cold-producing medium interlayer, adiabator layer from inside to outside,
Described cold-producing medium interlayer interior circulation has cold-producing medium, and temperature controls setting using outside water bath with thermostatic control；Described hydrate reaction kettle kettle
Internal portion is coated with titanium layer, is provided with refrigeration coil in reactor；Described hydrate reaction kettle kettle top flange is connected with kettle cover, institute
State kettle cover to be provided with gas emptying and collect valve, monitor the pressure sensor of gaseous pressure and difference in hydrate reaction kettle
The temperature sensor of gas phase temperature and liquidus temperature in detection hydrate reaction kettle；Described hydrate reaction kettle upper end is provided with solution
Spray equipment；Described hydrate reaction kettle lower end is provided with mechanical stirring device, gas feed, vacuum-pumping valve and with hydrate slurry
The hydrate slurry outlet of liquid heater connection；It is mounted with one-way cock at described gas feed；
Described data acquisition and processing unit include data collecting instrument, pass with the temperature that described data acquisition process instrument connects
Sensor and pressure sensor；Described temperature sensor be respectively used to monitor described gas cooler, hydrate reaction kettle liquid phase,
Hydrate slurry heater, the temperature of liquid chiller, described pressure sensor are used for monitoring described hydrate reaction kettle pressure；
Described gas boosting pump connects with hydrate reaction kettle gas feed via gas cooler；Described hydrate reaction
The gas collection valve that kettle kettle cover is provided with is connected with gas-drying apparatus and gas chromatograph；Described hydrate reaction kettle lower end sets
It is anti-that the outlet of some hydrate slurries is connected with hydrate slurry heater, liquid booster pump and liquid chiller, hydrate in turn
Answer the inlet that kettle upper end is provided with, form a loop.
Described hydrate reaction kettle is made up of high voltage bearing stainless steel, and described cold-producing medium interlayer interior circulation has cold-producing medium, right
In hydrate reaction kettle kettle, material is lowered the temperature or is heated up, and cooling and temperature-rise period and cryogenic temperature adopt exterior terminal to control
Set.
The adiabator layer of described hydrate reaction kettle wall, makes heat scatter and disappear as far as possible and reaches minimum.Described hydrate is anti-
Answer and in kettle, be provided with refrigeration coil, to increase the refrigerating capacity during hydrate reaction.
It is coated with titanium layer to increase wall hydrophobicity, it is to avoid hydrate slurry generates in reactor wall inside described kettle.
Described solution spraying device, the aqueous solution is uniformly sprayed into hydrate reaction kettle, and increase solution is connect with gas
Contacting surface is amassed.
Described hydrate reaction kettle side is provided with form, can monitor the whole process of hydrate reaction.
Described hydrate slurry heater is used for the hydrate slurry that heat resolve is derived from described hydrate reaction bottom portion,
Co after decomposition2Gas is discharged by valve, is used as the raw material of industry after collection, and the remaining aqueous solution is then increased by liquid booster pump
It is delivered to after pressure in liquid chiller and enter hydrate reaction kettle after being cooled to reactor setting temperature.
Described gas cooler, hydrate reaction kettle, hydrate slurry heater and liquid chiller pass through constant temperature respectively
Temperature controlled water baths.
The present invention also provides one kind based on co in hydrate separation biogas2Method, using said apparatus, including following
Step:
A, raw material biogas is pressurized to 2-5mpa by gas boosting pump, and is passed through gas cooling chamber and be cooled to 273-
280k, then gas is passed through in the hydrate reaction kettle after vacuumizing, and ensures that gas does not flow back by unidirectional stop valve, in kettle
Temperature controls between 273-280k by water bath with thermostatic control, and Stress control is between 2-5mpa；Meanwhile, needed for hydrate being generated
Mass concentration be 0-40% the aqueous solution containing accelerator uniformly spray in reactor gas phase by spray equipment, open react
Kettle lower mechanical agitating device, promotes the aqueous solution and gas to be fully contacted generation hydrate reaction, the total amount of described spray solution
Reach the volume of reactor 3/4；
B, after hydrate reaction terminates, discharge the hydrate slurry generating, and heated by hydrate slurry heater
Decompose the hydrate generating, co hydrate being collected by valve2Discharge Deng sour gas, reclaim the aqueous solution obtaining simultaneously
It is sent to recycling in hydrate reaction kettle again after being sent to cooling in liquid chiller after liquid booster pump supercharging；Hydration
In thing reactor, residual gas, after drying, uses chromatographic gas component, if meeting with gas requirement, directly defeated
Go out, if not meeting, recirculating and being passed through the reaction of hydrate reaction kettle until meeting the requirements.
The total amount of described spray solution reaches the volume of reactor 3/4 so that the density of hydrate slurry declines, most useful for
co2The separation of gas, and transporting most useful for hydrate slurry, it is to avoid hydrate lumps gathering in reactor.
Beneficial effects of the present invention are as follows:
1st, the internal titanizing layer of described hydrate reaction kettle, it is to avoid hydrate is more and more gathered on reactor wall,
Solve the problems, such as that in conventional hydrate separation gas, hydrate slurry is assembled in a kettle. thus circulating not smooth；
2nd, hydrate reaction kettle of the present invention adopts external jacket refrigeration and inner disk control cold dual refrigeration method, simultaneously outer
Bread covers adiabator layer, and wherein external jacket and internal coil pipe freeze respectively, both can guarantee that big during hydrate reaction
Refrigerating environment, reduces heat and scatters and disappears, hydrate reaction temperature in the kettle can be made again uniform.
3rd, hydrate reaction bottom portion is provided with mechanical stirring device, and reactor top is provided with solution spraying device, will stir
Combine with spray, increase the contact area of gases at high pressure and the aqueous solution as far as possible, promote the generation of hydrate.
4th, hydrate generates the required aqueous solution containing accelerator is to react, with water, the object that can generate half Study of Clathrate Hydrates
The mixed aqueous solution of molecule and surfactant, this mixed solution can effectively reduce temperature required for hydrate generates and
Pressure condition is moreover it is possible to promote the generation of hydrate and the separation of gas, and does not cause big harm, not corrosion reaction to environment
Kettle.
5th, the hydrate slurry generating after hydrate reaction discharges reactor by valve, and being then passed through heating makes it separate
Become gas and the aqueous solution, and reclaimed respectively, gas can serve as the raw material of industry, the aqueous solution can repeat to recycle.
6th, hydrate reaction kettle gas vent connects gas chromatograph, at any time ch in monitoring gas reactor4, co2And h2s
Content, as long as gas component reaches the standard with gas, gas can be exported at any time.
In a word, the application structure is simple, and technique is simpler, more energy efficient, for biogas (co2Comparision contents are high) separation effect
Fruit is more preferably.
Brief description:
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the profile of hydrate reaction kettle；
Wherein, 1. gas boosting pump, 2. pressure gauge, 3. temperature sensor, 4. water bath with thermostatic control, 5. gas cooler, 6. single
To stop valve, 7. pressure sensor, 8. temperature sensor, 9. temperature sensor, 10. data collecting instrument, 11. hydrate reactions
Kettle, 12. forms, 13. vavuum pump 14. feed tube, 15. waters bath with thermostatic control, 16. hydrate slurry heaters, 17. waters bath with thermostatic control, 18.
Temperature sensor, 19. liquid booster pumps, 20. liquid chillers, 21. temperature sensors, 22. gas-drying apparatus, 23. gas phase colors
Spectrometer, 24. cold-producing mediums are imported and exported, 25. adiabator layers, and 26. refrigeration coils are imported and exported, 27. reactor supports, and 28. machineries stir
Mix device, 29. refrigeration coils, 30. cold-producing medium interlayers, 31. solution spraying devices, 32. adpting flanges；V1-v10. valve.
Specific embodiment:
The following is and the present invention is further illustrated, rather than limitation of the present invention.
One kind is based on co in hydrate separation biogas2Device, as shown in figure 1, including for being pressurized to biogas
The gas boosting pump 1 of predetermined pressure, the gas cooler 5 being cooled to predetermined temperature, hydrate reaction kettle 11, hydrate slurry add
Hot device 16, liquid booster pump 19, liquid chiller 20, gas chromatograph 23, data acquisition and processing unit and valve v1-
V10 and pipeline；
As shown in Fig. 2 described hydrate reaction kettle 11 wall, using jacket structured, is followed successively by cold-producing medium interlayer from inside to outside
30th, adiabator layer 25, described cold-producing medium interlayer 30 interior circulation has cold-producing medium, and cryogenic temperature is controlled using outside water bath with thermostatic control 15
It is fixed to set up；It is coated with titanium layer inside described hydrate reaction kettle 11 kettle, in reactor, be provided with refrigeration coil 29；Described hydrate is anti-
Kettle 11 kettle top is answered to be connected with kettle cover by adpting flange 32 flange, described kettle cover is provided with gas emptying and collects valve
V7, monitoring hydrate reaction kettle 11 in gaseous pressure pressure sensor 7 and respectively detection hydrate reaction kettle 11 in gas phase temperature
Degree and the temperature sensor 8,9 of liquidus temperature；Described hydrate reaction kettle 11 upper end is provided with solution spraying device 31；Described hydration
Thing reactor 11 lower end is provided with mechanical stirring device 28, gas feed, vacuum-pumping valve and connects with hydrate slurry heater 16
Logical hydrate slurry outlet；It is mounted with one-way cock 6 at described gas feed；
Described data acquisition and processing unit include data collecting instrument 10, the temperature connecting with described data acquisition process instrument 10
Degree sensor 3,8,9,18,21 and pressure sensor 7；Described temperature sensor 3,8,9,18,21 is respectively used to monitor described gas
Body cooler 5, hydrate reaction kettle 11 liquid phase, hydrate slurry heater 16, the temperature of liquid chiller 20；
Described gas boosting pump 1 connects with hydrate reaction kettle 11 gas feed via gas cooler 5；Described hydrate
The gas collection valve that reactor 11 kettle cover is provided with is connected with gas-drying apparatus 22 and gas chromatograph 23；Described hydrate is anti-
The hydrate slurry outlet that kettle 11 lower end is provided with is answered to be connected with hydrate slurry heater 16, liquid booster pump 19 and liquid in turn
The inlet that cooler 20, hydrate reaction kettle 11 upper end are provided with, forms a loop.
It is based on co in hydrate separation biogas using said apparatus2Method as follows:
1. open valve v1, unstripped gas is passed through in booster pump 1 and is pressurized to certain pressure (according to ch in raw material biogas4's
Content is different, and pressure limit is between 2-5mpa), pressure value is read by pressure gauge 2.It is then turned on valve v2, will increase
Unstripped gas after pressure is passed through in gas cooler 5 and is cooled to 273-280k, and gas cooler 5 is lowered the temperature by water bath with thermostatic control 4, temperature
Controlled by temperature sensor 3.
2. open valve v3, using vavuum pump 13, hydrate reaction kettle is vacuumized, by the high pressure feed warp after cooling
Unidirectional stop valve 6 is passed through in hydrate reaction kettle 11, will react kettle temperature using refrigeration coil 26 in water bath with thermostatic control 15 and reactor
Degree is reduced to suitable temperature (temperature range is between 273-280k), and in course of reaction, reacting kettle inner pressure numerical value is passed by pressure
Sensor 7 gathers, and gas phase temperature and liquidus temperature are gathered by temperature sensor 8 and 9 respectively, and collection numerical value passes through data collecting instrument 10
Collect.
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 high pressure feed be fully contacted reaction and generate hydrate.
4. after hydrate reaction terminates, when that is, pressure sensor numerical value 7 no longer changes, open valve v4, will give birth to
The hydrate slurry becoming is transported in solution heater 16 and is heated, and solution heater temperature is controlled by water bath with thermostatic control 17, sets
In 300k, decompose hydrate slurry with abundant.Co after decomposition2Gas is discharged by valve v5, is collected, and can use further
Make the raw material of industry.The remaining aqueous solution is delivered in liquid chiller 20 after being then pressurized by liquid booster pump 19 and is cooled to
Continue through valve v6 after reactor setting temperature and feed tube 14 enters and participates in reaction in hydrate reaction kettle.
5. open valve v8, the purification gas in reactor is dried through drier 22, then utilize gas phase color
Spectrometer 23 carries out constituent analysis to gas, works as ch4When constituent content reaches requirement, open valve v9, gas is passed through three-way valve
V10 exports, and when foreign gas content is not up to standard, is then circulated gas again.
Embodiment 1
Take raw material gas sample, wherein ch4Content is 60%, co2Content is 40%, chooses the sds water that mass concentration is 300ppm
Solution, temperature of reaction kettle is 278k, when pressure is 5mpa, after reaction 30min, ch in reactor gas phase4Content bring up to
90.8%, co2Content be 9.2%, then after one cycle, ch in reactor gas phase4Content be 97.1%, co2Contain
Measure as 2.9%.
Embodiment 2
Take raw material gas sample, wherein ch4Content is 50%, co2Content is 50%, chooses the tbab that mass concentration is 0.05%
The aqueous solution, temperature of reaction kettle is 276k, when pressure is 3.5mpa, after reaction 30min, ch in reactor gas phase4Content be
88.8%, co2Content be 11.2%, after decomposition of hydrate, unstripped gas again through 2 times circulation after, ch in reactor gas phase4
Content be 95.3%, co2Content be 4.7%.
Embodiment 3
Take raw material gas sample, wherein ch4Content is 40%, co2Content is 59%, h2S content is 1%, chooses mass concentration and is
The sds mixed aqueous solution of 1% thf and 100ppm, temperature of reaction kettle is 278k, and pressure is 2.5mpa, after reaction 1h, reactor
Ch in interior gas phase4Content is 85.5%, co2Content is 13.9%, h2S content is 0.6%, after 3 circulations, ch4Content is
95.2%, co2Content is 4.2%, h2S content is 0.4%.
Claims (3)
1. one kind is based on co in hydrate separation biogas2Device it is characterised in that including pre- for being pressurized to biogas
The gas boosting pump (1) of constant-pressure, the gas cooler (5) being cooled to predetermined temperature, hydrate reaction kettle (11), hydrate slurry
Liquid heater (16), liquid booster pump (19), liquid chiller (20), gas chromatograph (23), data acquisition and processing unit
And valve (v1-v10) and pipeline；
Described hydrate reaction kettle (11) wall, using jacket structured, is followed successively by cold-producing medium interlayer (30), thermal insulating material from inside to outside
The bed of material (25), described cold-producing medium interlayer (30) interior circulation has cold-producing medium, and cryogenic temperature is set using outside water bath with thermostatic control (15) control
Fixed；It is coated with titanium layer inside described hydrate reaction kettle (11) kettle, in reactor, be provided with refrigeration coil (29)；Described hydrate is anti-
Kettle (11) kettle top flange is answered to be connected with kettle cover, described kettle cover is provided with gas emptying and collects valve (v7), monitoring water
The pressure sensor (7) of the interior gaseous pressure of compound reactor (11) and respectively detection hydrate reaction kettle (11) interior gas phase temperature and
The temperature sensor (8,9) of liquidus temperature；Described hydrate reaction kettle (11) upper end is provided with solution spraying device (31)；Described water
Compound reactor (11) lower end is provided with mechanical stirring device (28), gas feed, vacuum-pumping valve and heats with hydrate slurry
The hydrate slurry outlet that device (16) connects；It is mounted with one-way cock (6) at described gas feed；
Described data acquisition and processing unit include data collecting instrument (10), pass with the temperature that described data collecting instrument (10) connects
Sensor (3,8,9,18,21) and pressure sensor (7)；It is described that described temperature sensor (3,8,9,18,21) is respectively used to monitoring
Gas cooler (5), hydrate reaction kettle (11) liquid phase, hydrate slurry heater (16), the temperature of liquid chiller (20)
Degree；Described gas boosting pump (1) connects with hydrate reaction kettle (11) gas feed via gas cooler (5)；Described hydration
The gas collection valve that thing reactor (11) kettle cover is provided with is connected with gas-drying apparatus (22) and gas chromatograph (23)；Described
The pipeline through being provided with three-way valve (v10) for the gas chromatograph (23) also connects with gas boosting pump (1), forms a loop；Described
The hydrate slurry outlet that hydrate reaction kettle (11) lower end is provided with is connected with hydrate slurry heater (16) in turn, liquid increases
The inlet that press pump (19) and liquid chiller (20), hydrate reaction kettle (11) upper end are provided with, forms a loop.
2. co in the separation biogas based on hydrate according to claim 12Device it is characterised in that described hydrate
Reactor side is provided with form.
3. one kind is based on co in hydrate separation biogas2Method it is characterised in that utilize claim 1 or 2 described devices,
Comprise the following steps:
A, biogas is pressurized to 2-5mpa by gas boosting pump, and is passed through gas cooling chamber and be cooled to 273-280k, then will
Gas is passed through in the hydrate reaction kettle after vacuumizing, and ensures that gas does not flow back by unidirectional stop valve, temperature in the kettle passes through perseverance
Tepidarium controls between 273-280k, and Stress control is between 2-5mpa；Meanwhile, hydrate is generated required mass concentration
Uniformly sprayed in reactor gas phase by spray equipment for the 0-40% aqueous solution containing accelerator, open reactor lower mechanical
Agitating device, promotes the aqueous solution and gas to be fully contacted generation hydrate reaction, the total amount of described spray solution reaches reactor
3/4 volume；
B, after hydrate reaction terminates, discharge generate hydrate slurry, and pass through hydrate slurry heater heat resolve
The hydrate generating, co hydrate being collected by valve2Sour gas is discharged, and reclaims the aqueous solution obtaining through liquid simultaneously
It is sent to recycling in hydrate reaction kettle again after being sent to cooling in liquid chiller after the supercharging of body booster pump；Hydrate reaction
In kettle, residual gas, after drying, uses chromatographic gas component, if meeting with gas requirement, directly exports, if not
Meet, recirculate and be passed through the reaction of hydrate reaction kettle until meeting the requirements.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410586780.2A CN104403711B (en) | 2014-10-28 | 2014-10-28 | Method and apparatus for separating CO2 in biogas based on hydrate process |
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| CN108722149B (en) * | 2017-04-13 | 2021-05-04 | 中国石油化工股份有限公司 | Method and device for treating acid gas |
| CN108722135B (en) * | 2017-04-13 | 2021-03-02 | 中国石油化工股份有限公司 | Acid gas combined treatment process and system |
| CN108722140B (en) * | 2017-04-13 | 2021-03-02 | 中国石油化工股份有限公司 | Acid gas treatment process and system |
| CN107325852A (en) * | 2017-05-31 | 2017-11-07 | 常州大学 | A kind of method and its device based on hydrate processing cultivation excreta |
| CN109541084B (en) * | 2018-11-28 | 2021-11-16 | 湖北航天化学技术研究所 | Device for dynamically analyzing and detecting gas-phase product |
| CN109758997B (en) * | 2018-12-28 | 2021-03-09 | 中国科学院广州能源研究所 | Hydrate rapid reaction system based on fluidized bed |
| CN110205173A (en) * | 2019-07-03 | 2019-09-06 | 中国科学院武汉岩土力学研究所 | A kind of gas hydrate injection synthetic test system |
| 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 |
| CN110577851A (en) * | 2019-09-12 | 2019-12-17 | 华南理工大学 | device and method for quickly and continuously hydrating and separating coal bed gas |
| 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 |
| CN111650353A (en) * | 2020-06-28 | 2020-09-11 | 中国华能集团有限公司 | Gas separation experimental system and method by hydrate method |
| CN114352272B (en) * | 2020-09-28 | 2023-07-25 | 中国石油天然气股份有限公司 | Three-dimensional experimental system for three-dimensional loading simulation of hydrate reservoir yield increase transformation and exploitation |
| CN115041004A (en) * | 2022-06-20 | 2022-09-13 | 西南石油大学 | CO capture and separation by hydrate method 2 Method and dynamics monitoring device |
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| JP2004107468A (en) * | 2002-09-18 | 2004-04-08 | Jfe Engineering Kk | Method and equipment for producing gas clathrate |
| CN100493672C (en) * | 2006-11-10 | 2009-06-03 | 中国科学院广州能源研究所 | Hydrate process and apparatus for separating gas mixture continuously |
| CN101530719B (en) * | 2008-03-13 | 2011-11-30 | 中国石油大学(北京) | Method and device for low-pressure processing of coal bed gas |
| CN102678090A (en) * | 2011-03-16 | 2012-09-19 | 中国海洋石油总公司 | Three-dimensional synthesizing and mining simulation device for natural gas hydrate |
| CN103278374B (en) * | 2013-06-14 | 2015-04-22 | 中国科学院广州能源研究所 | In situ Raman analysis device for representing hydrate and in situ Raman analysis method of hydrate sample |
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