CN106866587A - A kind of process for separating and recovering of 1,4 butanediol dehydrogenation gamma butyrolactone hydrogen rich off gas - Google Patents
A kind of process for separating and recovering of 1,4 butanediol dehydrogenation gamma butyrolactone hydrogen rich off gas Download PDFInfo
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Abstract
The invention discloses a kind of process for separating and recovering of Isosorbide-5-Nitrae butanediol dehydrogenation gamma butyrolactone hydrogen rich off gas, hydrogen rich off gas obtain the hydrogen product of 99.9~99.99v% of purity through cooling I, compression, cooling II, temp.-changing adsorption.After the condensate liquid mixing that said process is separate, tetrahydrofuran is reclaimed using two tower joint rectifying, product purity is more than 99.95wt%；Gamma butyrolactone is reclaimed using rectification under vacuum, product purity is more than 99.9wt%.The technique farthest can separate and recover the useful constituents such as the hydrogen in hydrogen rich gas, tetrahydrofuran, gamma butyrolactone, hydrogen is more than 99% with tetrahydrofuran yield, gamma butyrolactone yield is more than 95%, has the advantages that the rate of recovery high, good product quality, the three wastes are few.
Description
Technical field
The invention belongs to industrial tail gas recycling field, and in particular to a kind of BDO dehydrogenation gamma-butyrolacton
During produce hydrogen rich off gas process for separating and recovering.
Background technology
Gamma-butyrolacton is important organic synthesis raw material and fine solvent, for synthesis of pyrrolidine ketone series of products, ring third
Amine, acetyl group gamma-butyrolacton and spices, medicine intermediate etc., it is also possible to make organic polymer reaction, the solvent of Dyestuff synthesis.
BDO dehydrogenation is one of main method of production gamma-butyrolacton, and BDO is made in Cu-series catalyst
Under, under 180~250 DEG C and condition of normal pressure, dehydrogenation obtains gamma-butyrolacton.This process meeting discharge unit hydrogen rich off gas, wherein
Density of hydrogen 95-99v% (percent by volume), also part tetrahydrofuran, gamma-butyrolacton, butanol and water.The existing place of the gas
Reason approach generally has two kinds, and one is that, by torch burning disposal, the method is a kind of wasting of resources.Two are returned by pressure-variable adsorption
Receive hydrogen, but the method can not reclaim the organic component in tail gas, especially tetrahydrofuran, gamma-butyrolacton both have
The component of larger economic worth.And, using existing pressure swing adsorption technique reclaim hydrogen, due to adsorbent to tetrahydrofuran,
The absorption affinity of gamma-butyrolacton is stronger, and adsorbent can not be desorbed completely under normal temperature, influences adsorption effect and sorbent life.
This patent provides a kind of new hydrogen rich off gas process for separating and recovering, and the technique can not only be reclaimed to hydrogen,
High-purity hydrogen is prepared, tetrahydrofuran therein, gamma-butyrolacton high-purity recovery can also be carried out in addition, recovery value is improved.
Because using temperature swing adsorption process, the complete desorption of adsorbent energy of adsorption, it is ensured that adsorption effect and sorbent life.The technique is normal
During operation, non-exhaust emission.After being reclaimed to organic matter, waste liquid amount also greatly reduces, and reduces pollution on the environment, is
A kind of environmentally friendly technique.
The content of the invention
Prior art reclaims the pressure swing adsorption technique that hydrogen rich off gas are used, and can only reclaim hydrogen, and adsorbent to four
Hydrogen furans, gamma-butyrolacton absorption affinity it is stronger, under normal temperature adsorbent can not desorption completely, cause sorbent life short, run
Effect on driving birds is not good, it is relatively costly.
A kind of problem that the present inventor exists for prior art, there is provided BDO dehydrogenation γ-fourth
The process for separating and recovering of lactone hydrogen rich off gas, the technique can simultaneously separate and recover hydrogen, tetrahydrofuran, three kinds of tools of gamma-butyrolacton
Commercially valuable exhaust gas composition, recovery purity is high, and uses temperature swing adsorption process, carries out high temperature regeneration to adsorbent, greatly
Big extension sorbent life.
A kind of process for separating and recovering of 1,4- butanediol dehydrogenations gamma-butyrolacton hydrogen rich off gas of the present invention is wrapped substantially
Following steps are included, the technological process that these steps can be combined shown in accompanying drawing of the present invention 1 is understood：
(1) I is cooled down：The hydrogen rich off gas unstripped gas that BDO dehydrogenation gamma-butyrolacton is produced is cooled to 5-15 DEG C,
Condensate liquid is separated by gas-liquid separator, separating liquid imports collecting tank, gas is for further processing.
(2) compress：The gas pressurized after I gas-liquid separations will be cooled down to 1.0~3.0MPa, the separating liquid obtained after compression is entered
Enter collecting tank, gas proceeds next step treatment.
(3) II is cooled down：Gas after step (2) is compressed is cooled to 5-15 DEG C again, will be condensed by gas-liquid separator
Liquid is separated, and separating liquid enters collecting tank, and gas phase enters temperature swing absorption unit.
(4) temp.-changing adsorption：The gas phase after cooling down II gas-liquid separations is carried out at absorption with adsorbent at 5 DEG C~15 DEG C
Reason, collects absorption residual gas and obtains high-purity hydrogen；After adsorbent adsorption saturation, 120~200 DEG C of solutions are heated to adsorbent
Absorption regeneration, the regeneration tail gas that desorption is produced are cooled to 5-15 DEG C into liquid, and collecting tank is entered by gas-liquid separator, adsorb
It is again introduced into coming into operation after agent cooling.
(5) tetrahydrofuran is reclaimed：The separating liquid that step (1)~(4) enter in collecting tank, is first mixed, and is entered back into often
The azeotropic mixture of pressure tower, atmospheric tower overhead extraction tetrahydrofuran and water, enters pressurizing tower after supercharging, and pressurizing tower overhead extraction is four
Hydrogen furans and the azeotropic mixture of water, return to atmospheric tower, and the tetrahydrofuran product of high-purity, atmospheric tower tower reactor are obtained from pressurizing tower tower reactor
Material enters vacuum tower.
(6) recovery of gamma-butyrolacton：Atmospheric tower kettle material enters vacuum tower, vacuum tower overhead extraction be water, butanol,
A small amount of gamma-butyrolacton and tetrahydrofuran, used as liquid waste processing, tower reactor obtains the gamma-butyrolacton product of high-purity.
Some specific embodiments of the invention, step (1), (3), the cooling described in (4) are carried out using chilled water.
Some specific embodiments of the invention, the pressure of the hydrogen rich off gas unstripped gas of step (1) is 10~30kPa,
30~50 DEG C of temperature, composition includes：Hydrogen 95-99v%, gamma-butyrolacton 0.05-0.2v%, tetrahydrofuran 0.3-3v%, butanol
0.05-0.2v%, water 0.4-2v%.
Step (2) compression compressor used is not limited to form, can reach the pressure effect, it is preferred to use reciprocal
Compressor.Further, the gas after cooling I gas-liquid separations first enters back into compressor compresses, such compressor after buffered tank
The pressure of entrance is relatively stable.
Preferably, the temp.-changing adsorption of step (4) uses isobaric variable temperature absorbing process.Whole recovery process can be ensured
Continuity and stability.It is simultaneously easily operated, can avoid introducing other impurities.
Step (4) heating adsorbent reactivation can use various methods, preferably, some specific embodiments of the invention
Adsorbent desorption is regenerated after raw material hydrogen rich off gas are heated into 160~220 DEG C.
Preferably, the adsorbent of step (4) is two in special typed active carbon, modified silica-gel, special-alumina, molecular sieve
Plant or various.
Preferably, step (5) atmospheric tower operating pressure be 0.01~0.05MPaG, pressurizing tower operating pressure be 0.5~
0.8MPaG。
Preferably, step (6) vacuum tower operating pressure is -0.09~-0.05MPaG.
Preferably, step (5) atmospheric tower reflux ratio is 1~3, pressurizing tower reflux ratio is 0.5~2.
Preferably, step (6) vacuum tower reflux ratio is 0.5~1.
The purity substantially 99.9v%~99.99v% of technique gained hydrogen of the invention, the purity can be according to actual need
The time of the amount by adjusting adsorbent and absorption is asked to realize.
Some specific embodiments of the invention, the tetrahydrofuran product purity obtained through step (5) is not less than
99.9%, more specifically, it is not less than 99.95wt%.The purity of the gamma-butyrolacton product obtained after step (6) treatment is not low
In 99.9wt%.And the rate of recovery is higher, hydrogen, tetrahydrofuran, the rate of recovery of gamma-butyrolacton are all higher than 95%.
Can be attached for conventional equipment according to the technique by device and its annexation involved by present invention process
To realize the effect, specific limitation is had no.
Wherein, step (4) temperature swing adsorption process can be according to actual conditions reasonable arrangement device and route, such as according to this
Some specific embodiments of invention, temperature swing adsorption system includes two absorbers, pre- absorber, regeneration hot-air heater, again
Angry cooler, gas-liquid separator and a series of program-controlled valves and pipeline etc..Gas phase after cooling II gas-liquid separations enters alternating temperature
Adsorption system, two-way is divided into through flow control circuit.Wherein one absorber is wherein directly removed all the way, wherein the adsorbent for loading
Tetrahydrofuran in gas, water, butanol and butyrolactone are absorbed, remaining hydrogen product is reached requirement.Another road elder generation
Into pre- absorber, another absorber is regenerated after being then heated to 180-220 DEG C by regenerating hot-air heater, adsorbed
Tetrahydrofuran, water, butanol etc. be just desorbed to form regeneration tail gas, then enter through regenerating after Gas Cooler is cooled to 5-15 DEG C
Gas-liquid separator, mainly contains tetrahydrofuran, water and butanol in separating liquid, into collecting tank, into step (5), separate gas and return to
The absorber for adsorbing.The adsorption column outlet temperature for being regenerated reaches 120-200 DEG C and regenerates completely, then uses unstripped gas
Cold blowing, cold blowing gas is heated to the 180-220 DEG C of pre- absorber of entrance through regenerating hot-air heater, and pre- absorber is regenerated.Absorption
Device outlet temperature reaches 5-15 DEG C i.e. cold blowing and completes, and can enter next adsorption cycle.Two adsorption tower rotations carry out absorption and
Regenerative process, i.e. in the state of a TSA adsorption tower is in absorption, another TSA adsorption tower is in regenerative process, absorption
Regenerated after agent adsorption saturation.Two adsorption tower operated in turn, reach the purpose of continuous processing gas.
The beneficial effects of the present invention are：
1st, simultaneous separation of hydrogen gas, γ-fourth from the hydrogen rich off gas of 1,4- butanediol dehydrogenation gamma-butyrolactons are provided first
The technique of lactone and tetrahydrofuran, fully recycles organic matter, while reducing the content of organic matter in waste liquid, turns waste into wealth,
Beneficial to environmental protection；
2nd, the process step of the invention is careful rigorous, and separation is targetedly designed according to three properties of composition to be recycled
And extraction step, mutually pollution had both been avoided, reduce wasting again, the rate of recovery is high；
3rd, technique recovery products obtained therefrom purity of the invention is high, can be come into operation without further treatment, with larger
Commercial value；
4th, the present invention uses temperature swing adsorption process, adsorbent is fully desorbed, and improves the adsorption efficiency of each adsorption cycle,
Extension sorbent life.
Brief description of the drawings
Fig. 1 is process for separating and recovering schematic flow sheet of the invention.
Specific embodiment
In order to preferably explain present disclosure, come to make further the present invention below by way of specific embodiment
It is bright, but should not be construed as protection scope of the present invention and be only limitted to this, all features disclosed in the content of the invention of the invention,
Disclosed all methods or during the step of, in addition to mutually exclusive feature and/or step, can be with any side
Formula is combined.Any feature disclosed in the present invention, unless specifically stated otherwise, can be by other replacements equivalent or with similar purpose
Feature is replaced.I.e., unless specifically stated otherwise, each feature be an example in a series of equivalent or similar characteristics and
.
Embodiment 1
The hydrogen rich off gas unstripped gas of table 1 constitutes (vol%)
| Component | Hydrogen | Tetrahydrofuran | Water | Butanol | Gamma-butyrolacton |
| V% | 98.66 | 0.49 | 0.63 | 0.09 | 0.13 |
Pressure 15kPa, 48 DEG C of temperature, flow 3000Nm3/h。
(1) I is cooled down：Hydrogen rich off gas are cooled to 15 DEG C through cooler, and gas-liquid separator is entered after cooling, isolate condensate liquid
16.64kg, wherein gamma-butyrolacton content 82.87wt%.Separating liquid removes collecting tank.
(2) compress：Gas phase after cooling I gas-liquid separations enters reciprocating compressor, through 4 grades of compressors to 2.2MPa.Compression
Machine stage separation liquid 14.82kg, primary aqueous, butanol and tetrahydrofuran remove collecting tank.
(3) II is cooled down：Compressor outlet gas enters cooler, and gas-liquid separation is entered after being water-cooled to 10 DEG C with freezing
Device, isolates condensate liquid 23.13kg, wherein content of tetrahydrofuran 58.55wt%.Separating liquid removes collecting tank.
(4) temp.-changing adsorption：Gas phase after cooling II gas-liquid separations enters temperature swing adsorption system.Tolerance 2971Nm3/ h, composition
For：Hydrogen 99.60v%, tetrahydrofuran 0.31v%, water 0.08v% and micro butanol and gamma-butyrolacton.Into temp.-changing adsorption
Gas be divided into two-way through flow control circuit first.TSA adsorption towers are wherein directly removed all the way, wherein the adsorbent for loading is by gas
Tetrahydrofuran, water, butanol and butyrolactone in body are absorbed, and obtain hydrogen product.Two adsorption tower rotations are adsorbed
And regenerative process, in the state of a TSA adsorption tower is in absorption, another TSA adsorption tower is in regenerative process.Adsorbent
Regenerated after adsorption saturation.Regeneration gas steam is heated to 160 DEG C, and adsorbent is heated into 120 DEG C, the tetrahydrochysene furan that will be adsorbed
Mutter, the desorption such as water, butanol, regeneration tail gas are cooled to 10 DEG C and enter gas-liquid separator, and separating liquid enters collecting tank.Isolate separation
Liquid 31.81kg, wherein content of tetrahydrofuran 93.26wt%.Then entered to 10 DEG C with the regeneration gas cold blowing processed through pre- adsorption tower
Row is adsorbed next time.Two adsorption tower operated in turn, reach the purpose of continuous processing gas.Temp.-changing adsorption outlet is produced for hydrogen
Product, flow 2959Nm3/ h, 10 DEG C of temperature, pressure 2.1MPa, hydrogen purity 99.98v%.
(5) tetrahydrofuran is reclaimed：Collecting tank mixed liquor 86.39kg/h, mixes laggard with the return material from pressurizing tower
Enter atmospheric tower.Atmospheric tower tower top pressure 0.02MPa, reflux ratio is 2, and overhead extraction is the azeotropic mixture of tetrahydrofuran and water, azeotropic
It is tetrahydrofuran 98.10wt% to constitute, water 1.90wt%, pressurized entrance pressurizing tower；Kettle material is sent into by pressure and depressurized
Tower.Pressurizing tower tower top pressure 0.60MPa, reflux ratio is 1.Overhead extraction is the azeotropic mixture of tetrahydrofuran and water, and azeotropic composition is
Tetrahydrofuran 97.56wt%, water 2.44wt%, return to atmospheric tower.Tower reactor is tetrahydrofuran product, flow 46.95kg/h, tetrahydrochysene
Furans purity 99.98wt%.
(6) gamma-butyrolacton is reclaimed：Atmospheric tower kettle material enters vacuum tower by pressure difference.Vacuum tower tower top pressure for-
0.08MPa, reflux ratio is 1.Tower reactor obtains gamma-butyrolacton product, flow 14.63kg/h, gamma-butyrolacton purity 99.9wt%.
Overhead extraction is the waste liquid containing organic matter, flow 24.65kg/h, wherein aqueous 61.52wt%, butanol 36.22wt%, butyrolactone
1.46wt%, tetrahydrofuran 0.80wt%.
The process closed operation of whole separation and recovery, non-exhaust emission.Hydrogen recovery rate 99.98%, the tetrahydrofuran rate of recovery
99.57%, the gamma-butyrolacton rate of recovery 97.60%.
Embodiment 2
The hydrogen rich off gas unstripped gas of table 2 constitutes (vol%)
| Component | Hydrogen | Tetrahydrofuran | Water | Butanol | Gamma-butyrolacton |
| V% | 98.75 | 0.60 | 0.50 | 0.05 | 0.10 |
Pressure 10kPa, temperature 45 C, flow 1400Nm3/h。
(1) I is cooled down：Hydrogen rich off gas are cooled to 10 DEG C through cooler, and gas-liquid separator is entered after cooling, isolate condensate liquid
6.09kg, wherein gamma-butyrolacton content 82.35wt%.Separating liquid removes collecting tank.
(2) compress：Cool down the gas phase after I gas-liquid separation and enter reciprocating compressor, through 4 grades of compressors to 2.5MPa.Compression
Machine stage separation liquid 4.72kg, removes collecting tank.
(3) II is cooled down：Compressor outlet gas enters cooler, and gas-liquid separator is entered after being cooled to 10 DEG C, isolates
Condensate liquid 16.02kg, wherein content of tetrahydrofuran 75.36wt%.Separating liquid removes collecting tank.
(4) temp.-changing adsorption：Similar to embodiment 1, enter temp.-changing adsorption tolerance 1382Nm3/ h, constitutes and is：Hydrogen
99.66v%, tetrahydrofuran 0.29v%, water 0.05v% and micro butanol and gamma-butyrolacton.Regeneration tail gas freezing water-cooled
But to 5 DEG C, separating liquid 13.52kg, wherein tetrahydrofuran 95.83wt% are isolated.Hydrogen product flow 1381Nm3/ h, temperature
10 DEG C, pressure 2.5MPa, hydrogen purity 99.95v%.
(5) tetrahydrofuran is reclaimed：Collecting tank mixed liquor 40.34kg/h, mixes laggard with the return material from pressurizing tower
Enter atmospheric tower.Atmospheric tower tower top pressure 0.01MPa, reflux ratio is 2.Overhead extraction is the azeotropic mixture of tetrahydrofuran and water, azeotropic
It is tetrahydrofuran 98.58wt% to constitute, water 1.42wt%, pressurized entrance pressurizing tower.Kettle material is sent into by pressure and depressurized
Tower.Pressurizing tower tower top pressure 0.70MPa, reflux ratio is 1.Overhead extraction is the azeotropic mixture of tetrahydrofuran and water, and azeotropic composition is
Tetrahydrofuran 98.08wt%, water 1.92wt%, return to atmospheric tower.Tower reactor is tetrahydrofuran product, flow 26.90kg/h, tetrahydrochysene
Furans purity 99.99wt%.
(6) gamma-butyrolacton is reclaimed：Atmospheric tower kettle material enters vacuum tower by pressure difference.Vacuum tower tower top pressure-
0.05MPa, reflux ratio is 1.Tower reactor obtains gamma-butyrolacton product, flow 5.12kg/h, gamma-butyrolacton purity 99.95wt%.
Overhead extraction is the waste liquid containing organic matter, flow 8.26kg/h, wherein aqueous 67.99wt%, butanol 28.01wt%, butyrolactone
3.19wt%, tetrahydrofuran 0.81wt%.
Hydrogen recovery rate 99.89%, the tetrahydrofuran rate of recovery 99.52%, the gamma-butyrolacton rate of recovery 95.17%.
Embodiment 3
The hydrogen rich off gas unstripped gas of table 3 constitutes (vol%)
| Component | Hydrogen | Tetrahydrofuran | Water | Butanol | Gamma-butyrolacton |
| V% | 99.15 | 0.45 | 0.30 | 0.05 | 0.05 |
Pressure 30kPa, 40 DEG C of temperature, flow 5000Nm3/h。
(1) I is cooled down：Hydrogen rich off gas are cooled to 5 DEG C through cooler, and gas-liquid separator is entered after cooling, isolate condensate liquid
14.56kg, wherein gamma-butyrolacton content 74.63wt%.Separating liquid removes collecting tank.
(2) compress：Cool down the gas phase after I gas-liquid separation and enter reciprocating compressor, through 3 grades of compressors to 1.1MPa.Compression
Condensation between machine level.
(3) II is cooled down：Compressor outlet gas enters cooler, is cooled to 5 DEG C and enters gas-liquid separator, isolates condensation
Liquid 30.80kg, wherein content of tetrahydrofuran 56.79wt%.Separating liquid removes collecting tank.
(4) temp.-changing adsorption：Enter temp.-changing adsorption tolerance 4978Nm3/ h, constitutes and is：Hydrogen 99.58v%, tetrahydrofuran
0.34v%, water 0.08v% and micro butanol and gamma-butyrolacton.Regeneration tail gas freezing is water-cooled to 5 DEG C, isolates separation
Liquid 57.21kg, wherein tetrahydrofuran 93.91wt%.Hydrogen product flow 4951Nm3/ h, 5 DEG C of temperature, pressure 1.0MPa, hydrogen
Purity 99.96v%.
(5) tetrahydrofuran is reclaimed：Collecting tank mixed liquor 102.58kg/h, mixes laggard with the return material from pressurizing tower
Enter atmospheric tower.Atmospheric tower tower top pressure 0.04MPa, reflux ratio is 1.5.Overhead extraction is the azeotropic mixture of tetrahydrofuran and water, altogether
Boiling composition is tetrahydrofuran 97.46wt%, water 2.54wt%, pressurized entrance pressurizing tower.Kettle material is sent into by pressure and subtracted
Pressure tower.Pressurizing tower tower top pressure 0.50MPa, reflux ratio is 1.Overhead extraction is the azeotropic mixture of tetrahydrofuran and water, azeotropic composition
It is tetrahydrofuran 96.62wt%, water 3.38wt%, returns to atmospheric tower.Tower reactor is tetrahydrofuran product, flow 71.08kg/h, four
Hydrogen furans purity 99.95wt%.
(6) gamma-butyrolacton is reclaimed：Atmospheric tower kettle material enters vacuum tower by pressure difference.Vacuum tower tower top pressure-
0.05MPa, reflux ratio is 0.5.Tower reactor obtains gamma-butyrolacton product, flow 11.09kg/h, gamma-butyrolacton purity
99.9wt%.Overhead extraction is the waste liquid containing organic matter, flow 19.36kg/h, wherein aqueous 62.01wt%, butanol
34.16wt%, butyrolactone 2.26wt%, tetrahydrofuran 1.57wt%.
Hydrogen recovery rate 99.87%, the tetrahydrofuran rate of recovery 98.61%, the gamma-butyrolacton rate of recovery 96.18%.
Claims (10)
1. a kind of process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas, it is characterised in that including following
Step：
(1) I is cooled down：The hydrogen rich off gas unstripped gas that BDO dehydrogenation gamma-butyrolacton is produced is cooled to 5-15 DEG C, is passed through
Gas-liquid separator separates condensate liquid, and separating liquid imports collecting tank, and gas is for further processing；
(2) compress：The gas pressurized after I gas-liquid separations to 1.0~3.0MPa will be cooled down, the separating liquid obtained after compression enters to be received
Collection tank, gas proceeds next step treatment；
(3) II is cooled down：Gas after step (2) is compressed is cooled to 5-15 DEG C again, is divided condensate liquid by gas-liquid separator
From separating liquid enters collecting tank, and gas phase enters temperature swing absorption unit；
(4) temp.-changing adsorption：The gas phase after cooling down II gas-liquid separations is carried out into adsorption treatment with adsorbent at 5 DEG C~15 DEG C, is received
Collection absorption residual gas obtains high-purity hydrogen；After adsorbent adsorption saturation, 120~200 DEG C of desorptions are heated to adsorbent
Regeneration, the regeneration tail gas that desorption is produced are cooled to 5-15 DEG C into liquid, and collecting tank, adsorbent drop are entered by gas-liquid separator
It is again introduced into coming into operation after temperature；
(5) tetrahydrofuran is reclaimed：The separating liquid that step (1)~(4) enter in collecting tank, is first mixed, and enters back into atmospheric tower,
The azeotropic mixture of atmospheric tower overhead extraction tetrahydrofuran and water, enters pressurizing tower after supercharging, and pressurizing tower overhead extraction is tetrahydrochysene furan
The azeotropic mixture muttered with water, returns to atmospheric tower, and the tetrahydrofuran product of high-purity, atmospheric tower kettle material are obtained from pressurizing tower tower reactor
Into vacuum tower；
(6) recovery of gamma-butyrolacton：Atmospheric tower kettle material enters vacuum tower, and vacuum tower overhead extraction is used as liquid waste processing, tower
Kettle obtains the gamma-butyrolacton product of high-purity.
2. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, the pressure of the hydrogen rich off gas unstripped gas of step (1) is 10~30kPa, 30~50 DEG C of temperature, and composition includes：Hydrogen 95-
99v%, gamma-butyrolacton 0.05-0.2v%, tetrahydrofuran 0.3-3v%, butanol 0.05-0.2v%, water 0.4-2v%.
3. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (2) compression compressor used is reciprocating compressor.
4. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (4) regenerates after raw material hydrogen rich off gas are heated into 160~220 DEG C to the adsorbent desorption.
5. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, the temp.-changing adsorption of step (4) uses isobaric variable temperature absorbing process.
6. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (4) described adsorbent is two kinds or many in special typed active carbon, modified silica-gel, special-alumina, molecular sieve
Kind.
7. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (5) atmospheric tower operating pressure is 0.01~0.05MPaG, pressurizing tower operating pressure is 0.5~0.8MPaG.
8. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (6) vacuum tower operating pressure is -0.09~-0.05MPaG.
9. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, it is special
Levy and be, step (5) atmospheric tower reflux ratio is 1~3, pressurizing tower reflux ratio is 0.5~2.
10. the process for separating and recovering of BDO dehydrogenation gamma-butyrolacton hydrogen rich off gas according to claim 1, its
It is characterised by, step (6) vacuum tower reflux ratio is 0.5~1.
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