CN1259120C - Pressure-varying adsorption method for concentrating and recovering chlorethylene from chlorethylene containing gas mixture - Google Patents
Pressure-varying adsorption method for concentrating and recovering chlorethylene from chlorethylene containing gas mixture Download PDFInfo
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- CN1259120C CN1259120C CN 200410040544 CN200410040544A CN1259120C CN 1259120 C CN1259120 C CN 1259120C CN 200410040544 CN200410040544 CN 200410040544 CN 200410040544 A CN200410040544 A CN 200410040544A CN 1259120 C CN1259120 C CN 1259120C
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Abstract
The present invention relates to a pressure-varying adsorption method for concentrating and recovering chloroethylene from mixed gas containing the chloroethylene, which has the aim of solving the problem that the purity of the chloroethylene recovered by the existing active carbon adsorption method and the film separation method is low. The method is carried out in a pressure-varying adsorption system of the circulating operation of at least two adsorption beds filling with adsorbent, and the circulation of adsorption beds every time comprises the following steps: adsorption, at least one-time pressure equalizing drop, displacement, reverse pressure release, evacuation, at least pressure equalizing boost or the displacement of exhaust gas, pressure boost and at least one-time pressure equalizing boost and final pressure boost; the present invention comprises the adsorption steps: absorbing the chloroethylene by the adsorbent so as to detain in the adsorption beds, obtaining purification gas and discharging the purification gas from the adsorption beds, improving the chloroethylene concentration in the adsorption beds by the displacement, carrying out desorption and regeneration for the adsorbent by the reverse pressure release and the evacuation, and discharging the high-content chloroethylene gas from the adsorption beds so as to carry out reutilization. The adsorbent is at least one of activated carbon, aluminum oxide and silica gel. The present invention is suitable for separating concentrating, and recovering the chloroethylene from the mixed gas, and is especially suitable for concentrating and recovering the chloroethylene from tail gas containing the chloroethylene in polyvinyl chloride production plants. The chloroethylene contents in the concentrated and recovered gas can reach 90 to 99%(volume %), and simultaneously, the recovery rate of the chloroethylene is larger than 95%.
Description
Technical field:
The present invention relates to purification, the recovery method of gaseous mixture, particularly adopt pressure swing adsorption method (PSA) to produce the method that concentrates and reclaim vinyl chloride the mist that tail gas or other contain vinyl chloride from polyvinyl chloride (PVC).
Background technology:
The polymerization tail gas of domestic polyvinyl chloride (PVC) industry production process need discharge unit vinyl-chloride-containing.Gas is roughly formed and is seen Table 1, as tail gas clean-up not being handled and directly discharged, not only can cause environmental pollution, and cause C
2H
3The Cl wasting of resources, the tail gas clean-up processing mode generally adopts organic solvent absorption process or activated carbon alternating temperature absorption method or membrane separation process in the polyvinyl chloride industry at present, the alternating temperature absorption method causes adsorbent loss and corrosive pipeline serious because of need adopt steam flush heating adsorbent bed, and owing to needs temperature to raise and reduce.Therefore cycle period is longer, the adsorbent large usage quantity.Adsorbent is shorter service life, and the vinyl chloride water content of Hui Shouing is bigger simultaneously, and content of vinylchloride is not high.Also there is the not high problem of content of vinylchloride of recovery in membrane separation process.
Summary of the invention:
Given this, the object of the present invention is to provide a kind of technological process simple, power consumption is few, the adsorbent long service life, the product gas recovery rate high the new method that concentrates and reclaim vinyl chloride.
Pressure swing adsorption method replacement active carbon alternating temperature absorption method, the concentrated purpose that reclaims vinyl chloride of membrane separation process realization that the present invention adopts selected adsorbent to cooperate displacement, find time.Concentrate higher the reaching more than 90% (the volume %) of content of vinylchloride of reclaiming, the rate of recovery Gao Keda of vinyl chloride is more than 95%.
Of the present inventionly concentrate and reclaim the vinyl chloride method and it is characterized in that in the pressure swing adsorption system of at least two adsorbent beds that are filled with adsorbent, each adsorbent bed of operation each time of system adsorbs (A) successively (to be adopted the vinyl chloride in the selected adsorbents adsorb mist and is trapped in the adsorbent bed, the Purge gas that obtains low content vinyl chloride is discharged system and emptying), at least once all pressure drops (ED), backflow accounts for the vinyl chloride product gas of volume 5%～80% and after pressurizeing adsorbent bed is replaced (RP), contrary put (D), (V) finds time, at least once all voltage rise (ER) or with displacement waste gas boost (R) add at least once all voltage rise replacements, the steps such as (FR) of finally boosting, to put and find time to obtain content be that the vinyl chloride gas of 90%～99% (volume %) returns the utilization of Production of PVC system recoveries by contrary.
In the above-mentioned pressure swing absorption process of the present invention, adsorptive pressure is greater than 0.15MPa, and evacuation pressure 0.01MPa～0.06MPa is against putting pressure 0.1MPa～0.15MPa, displacement step pressure 0.15MPa～1.0MPa.
The composition and the weight % of the adsorbent of selecting for use in the above-mentioned pressure swing absorption process of the present invention are as follows:
Activated alumina 0～100%
Silica gel 0～100%
Active carbon 0～60%
Above-mentioned pressure swing absorption process of the present invention, all pressure drops, equal voltage rise step are 1～5 time.
The present invention compares with existing active carbon alternating temperature absorption method, has following evident characteristic.
One, the present invention adopts pressure swing adsorption technique, it is simple to have technological process, the advantage that automaticity is high: the present invention is in 5 ℃～60 ℃ operations down of unstripped gas temperature, equipment is simple, regeneration of adsorbent beds does not need external heat source and low-temperature receiver, wholely concentrate, reclaim the vinyl chloride cyclic process and all realize automation mechanized operation, device start-stop car is very convenient.
Two, the present invention makes the vinyl chloride purity of recovery up to 90%～99% (volume %) after increasing replacement process.
Three, the present invention has the advantage of adsorbent long service life: generally can use more than 10 years.
Present device need not special material, solvent-free and auxiliary material consumption, and power consumption is low, and the device operation and maintenance cost is low.
The present invention is applicable to that Production of PVC tail gas or other contain the concentrated vinyl chloride that reclaims of mist of vinyl chloride.
Description of drawings:
Fig. 1 is one of process flow diagram of the present invention.
Fig. 2 is two of process flow diagram of the present invention.
Fig. 3 is three of process flow diagram of the present invention.
Fig. 4 is four of process flow diagram of the present invention.
Fig. 5 is five of process flow diagram of the present invention.
The specific embodiment:
Embodiment 1:
The Production of PVC tail gas composition of present embodiment sees Table 1.
Table 1 embodiment 1 polyvinyl chloride tail gas is formed (V%)
| Component | O 2 | N 2 | C 2H 3Cl |
| V％ | 5～10 | 70～85 | 8～20 |
Pressure swing adsorption system of the present invention is formed by connecting by adsorbent bed and a vinyl chloride surge tank, the surge tank of all calming the anger, displacement off-gas buffer tank, vavuum pump and a corresponding pipeline program-controlled valve of three filling 10% active carbon+60% silica gel+30% activated aluminas (weight %), sees Fig. 1.When system moves, control each sequencing valve by computer follow procedure (according to table 2 sequential).5 ℃ of temperature, pressure 0.4MPa polyvinyl chloride tail gas enter adsorbent bed through pipeline and sequencing valve, and the adsorbent of filling in the adsorbent bed is selected absorption and is trapped in the adsorbent bed other N the vinyl chloride in the tail gas
2, O
2Discharge emptying from the adsorbent bed top Deng gas, adsorption step adsorbs near stopping after saturated vinyl chloride absorption, open and all to press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out equal pressure drop, close after all pressure drop is finished and all press sequencing valve, open and after the displacement sequencing valve is forced into 0.35MPa with the compressed machine of vinyl chloride product gas that accounts for product gas long-pending 10% adsorbent bed is replaced to improve content of vinylchloride in the adsorbent bed, displacement waste gas enters the displacement off-gas buffer tank, after finishing, displacement closes the displacement sequencing valve, open the contrary sequencing valve of putting and carry out contrary strideing suddenly, contrary putting closed the contrary sequencing valve of putting after finishing, the unlatching sequencing valve of finding time is found time evacuation pressure 0.01MPa to adsorbent bed.Close the sequencing valve of finding time after finding time to finish, content is the vinyl chloride of 95-98% (volume %) in contrary venting and the exhaust, and output is out-of-bounds recycled as vinyl chloride product gas.And then unlatching displacement sequencing valve utilization displacement waste gas boosts to the adsorbent bed of vacuum state, boost and close the displacement sequencing valve after finishing, open and all to press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out equal voltage rise, close after all voltage rise is finished and all press sequencing valve, unlatching pressurising sequencing valve utilization absorption waste gas is pressurized to the adsorptive pressure difficulty to adsorbent bed and enters next working cycles fully.
Table 2 embodiment 1 pressure-swing absorption apparatus sequencing valve time-scale
| Divide the cycle | 1 | 2 | 3 | ||||||||||||||||
| The A tower | A | ED | RP | D | V | R | ER | FR | |||||||||||
| The B tower | V | R | ER | FR | A | ED | RP | D | V | ||||||||||
| The C tower | ED | RP | D | V | R | ER | FR | A | |||||||||||
Embodiment 2:
The Production of PVC tail gas composition of present embodiment sees Table 3.
Table 3 embodiment 2 polyvinyl chloride tail gas are formed (V%)
| Component | O 2 | N 2 | C 2H 3Cl |
| V％ | 5 | 65 | 30 |
Pressure swing adsorption system of the present invention is formed by connecting by four adsorbent bed and a vinyl chloride surge tank, the surge tank of all calming the anger, vavuum pump and corresponding pipeline program-controlled valves that load 70% silica gel+30% activated aluminas (weight %), shows as Fig. 2.
During the native system operation, control each sequencing valve by computer follow procedure (according to table 4 sequential).Temperature is that 40 ℃, pressure are that the polyvinyl chloride tail gas of 0.6MPa enters adsorbent bed through pipeline and sequencing valve, and the adsorbent of filling is selected absorption and is trapped in the adsorbent bed other N the vinyl chloride in the tail gas in the adsorbent bed
2, O
2Discharge emptying from the adsorbent bed top Deng gas, adsorption step stops absorption when saturated in vinyl chloride absorption, carry out equal pressure drop by all pressing sequencing valve and pipeline to be communicated with the surge tank of all calming the anger, close after all pressure drop is finished and all press sequencing valve, open the displacement sequencing valve, after being forced into 0.20MPa with the compressed machine of vinyl chloride product gas of 5% (volume %) adsorbent bed is replaced, to improve content of vinylchloride in the adsorbent bed.The displacement exhaust emission system mixes back emptying with absorption waste gas, displacement is closed the displacement sequencing valve after finishing, and opens the contrary sequencing valve of putting and carries out contraryly strideing suddenly, and contrary putting closed the contrary sequencing valve of putting after finishing, the unlatching sequencing valve of finding time is found time evacuation pressure 0.035MPa to adsorbent bed.Close the sequencing valve of finding time after finding time to finish, content is that the vinyl chloride of 95～98% (volume %) is as out-of-bounds recycling of vinyl chloride product gas output in contrary venting and the exhaust.Open and all to press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out equal voltage rise, close after all voltage rise is finished and all press sequencing valve, open the utilization of pressurising sequencing valve and adsorb waste gas and adsorbent bed is finally boosted to the adsorptive pressure preparation enter next working cycles.
Table 4 embodiment 2 pressure-swing absorption apparatus sequencing valve time-scales
| Divide the cycle | 1 | 2 | 3 | 4 | ||||||||||||
| The A tower | A | ED | RP | D | V | ER | FR | |||||||||
| The B tower | V | FR | A | ED | R | D | V | |||||||||
| The C tower | RP | D | V | ER | FR | A | ED | RP | ||||||||
| The D tower | ED | RP | D | V | ER | FR | A | |||||||||
Embodiment 3:
The Production of PVC tail gas composition of present embodiment sees Table 5.
Table 5 embodiment 3 polyvinyl chloride tail gas are formed (V%)
| Component | O 2 | N 2 | C 2H 3Cl |
| V％ | 5 | 70 | 25 |
Pressure swing adsorption system of the present invention is formed by connecting by six adsorbent bed and a vinyl chloride surge tank, the surge tank of all calming the anger, a vavuum pump and corresponding pipeline program-controlled valves that load 10% active carbon+90% silica gel (weight %), shows as Fig. 3.
During the native system operation, control each sequencing valve by computer follow procedure (according to table 6 sequential).The polyvinyl chloride tail gas of 25 ℃ of temperature, pressure 0.8MPa enters adsorbent bed through pipeline and sequencing valve, and the adsorbent of filling is selected absorption and is trapped in the adsorbent bed other N the vinyl chloride in the tail gas in the adsorbent bed
2, O
2Discharge emptying from the adsorbent bed top Deng gas, adsorption step adsorbs near stopping after saturated vinyl chloride absorption, by all pressing sequencing valve and another adsorbent bed to carry out once all pressure drops, one equal pressure drop is finished and is closed and all presses sequencing valve, opening with the tank connected sequencing valve of buffering of all calming the anger makes the adsorbent bed and the surge tank of all calming the anger carry out all pressure drops second time, close after all pressure drop is finished and all press sequencing valve, open and after the displacement sequencing valve is forced into 0.35MPa with the compressed machine of vinyl chloride product gas of 25% (volume %) adsorbent bed to be replaced with content of vinylchloride in the raising adsorbent bed, the displacement exhaust emission system mixes back emptying with absorption waste gas, after finishing, displacement closes the displacement sequencing valve, open the contrary sequencing valve of putting and carry out contrary strideing suddenly, contrary putting closed the contrary sequencing valve of putting after finishing, the unlatching sequencing valve of finding time is found time evacuation pressure 0.025MPa to adsorbent bed.Close the sequencing valve of finding time after finding time to finish, content is that the vinyl chloride of 97%～99% (volume %) is as out-of-bounds recycling of vinyl chloride product gas output in contrary venting and the exhaust.Open and all to press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out the equal voltage rise of secondary, close after all voltage rise is finished and all press sequencing valve, open all pressures sequencing valve that links to each other with another adsorbent bed again, carry out once all voltage rises, unlatching pressurising sequencing valve utilization absorption waste gas is pressurized to adsorptive pressure to adsorbent bed and prepares to enter next working cycles.
Present embodiment has adopted six flow processs, and any step all has two adsorbent beds to be in adsorption step, and therefore the disposal ability to polyvinyl chloride tail gas can reach 2000Nm more greatly
3More than/the h.
Table 6 embodiment 3 pressure-swing absorption apparatus program valve time-scales
| 1 | 2 | 3 | 4 | 5 | 6 | ||||||||||||||||||
| A | A | ED1 | ED2 | RP | D | V | ER2 | ER1 | FR | ||||||||||||||
| ER1 | FR | A | A | ED1 | ED2 | RP | D | V | ER2 | ||||||||||||||
| V | ER2 | ER1 | FR | A | A | ED1 | ED2 | RP | D | V | |||||||||||||
| RP | D | V | ER2 | ER1 | FR | A | A | ED1 | ED2 | RP | |||||||||||||
| ED1 | ED2 | RP | D | V | ER2 | ER1 | FR | A | A | ||||||||||||||
| A | ED1 | ED2 | RP | D | V | ER2 | ER1 | FR | A | ||||||||||||||
Embodiment 4:
The Production of PVC tail gas composition of present embodiment sees Table 7.
Table 7 embodiment 4 polyvinyl chloride tail gas are formed (V%)
| Component | O 2 | N 2 | C 2H 3Cl |
| V％ | 1 | 60 | 39 |
Pressure swing adsorption system of the present invention is formed by connecting by four adsorbent bed and a vinyl chloride surge tank, the surge tank of all calming the anger, a vavuum pump and corresponding pipeline program-controlled valves that load silica gel, shows as Fig. 4.
During the native system operation, control each sequencing valve by computer follow procedure (according to table 8 sequential).Temperature is that 40 ℃, pressure are that the polyvinyl chloride tail gas of 0.6MPa enters adsorbent bed through pipeline and sequencing valve, and the adsorbent of filling is selected absorption and is trapped in the adsorbent bed other N the vinyl chloride in the tail gas in the adsorbent bed
2, O
2Discharge emptying from the adsorbent bed top Deng gas, adsorption step stops absorption when saturated in vinyl chloride absorption, carry out equal pressure drop by all pressing sequencing valve and pipeline to be communicated with the surge tank of all calming the anger, close after all pressure drop is finished and all press sequencing valve, open the displacement sequencing valve, after being forced into 0.15MPa with the compressed machine of vinyl chloride product gas of 15% (volume %) adsorbent bed is replaced, to improve content of vinylchloride in the adsorbent bed, the displacement exhaust emission system mixes emptying afterwards with absorption waste gas.Displacement is closed the displacement sequencing valve after finishing, and opens the contrary sequencing valve of putting and carries out contraryly strideing suddenly, and contrary putting closed the contrary sequencing valve of putting after finishing, and opens the sequencing valve of finding time adsorbent bed is found time, and evacuation pressure is about 0.06MPa.Close the sequencing valve of finding time after finding time to finish, content is that the vinyl chloride of 90%～98% (volume %) is as out-of-bounds recycling of vinyl chloride product gas output in contrary venting and the exhaust.Open and all to press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out equal voltage rise, close after all voltage rise is finished and all press sequencing valve, open the utilization of pressurising sequencing valve and adsorb waste gas and adsorbent bed is finally boosted to the adsorptive pressure preparation enter next working cycles
Table 8 embodiment 4 pressure-swing absorption apparatus sequencing valve time-scales
| Divide the cycle | 1 | 2 | 3 | 4 | |||||||||||||
| The A tower | A | ED | RP | D | V | ER | FR | ||||||||||
| The B tower | V | ER | FR | A | ED | RP | D | V | |||||||||
| The C tower | RP | D | V | ER | FR | A | ED | RP | |||||||||
| The D tower | ED | RP | D | V | ER | FR | A | ||||||||||
Embodiment 5:
The polyvinyl chloride tail gas composition of present embodiment sees Table 9.
Table 9 embodiment 5 polyvinyl chloride tail gas are formed (V%)
| Component | O 2 | N 2 | C 2H 3Cl |
| V％ | 0.5 | 55 | 44.5 |
Pressure swing adsorption system of the present invention is formed by connecting by four adsorbent bed and a product gas surge tank, the surge tank of all calming the anger, vavuum pump and corresponding pipeline program-controlled valves that are filled with silica gel, shows as Fig. 5.
During the native system operation, control each sequencing valve by computer follow procedure (according to table 10 sequential), temperature is that 40 ℃, pressure are that the polyvinyl chloride tail gas of 1.2MPa enters adsorbent bed through pipeline and sequencing valve, the adsorbent of filling is selected absorption and is trapped in the adsorbent bed other N the vinyl chloride in the tail gas in the adsorbent bed
2, O
2Discharge emptying from the adsorbent bed top Deng gas, adsorption step stops absorption when saturated in vinyl chloride absorption.Carry out equal pressure drop by all pressing sequencing valve and pipeline to be communicated with the surge tank of all calming the anger, close after all pressure drop is finished and all press sequencing valve, open the displacement sequencing valve, after being forced into 1.0MPa with the compressed machine of vinyl chloride product gas of 15% (volume %) adsorbent bed is replaced, to improve content of vinylchloride in the adsorbent bed, the displacement exhaust emission system mixes back emptying with absorption waste gas, after finishing, displacement closes the displacement sequencing valve, open the contrary sequencing valve of putting and carry out contrary strideing suddenly, contrary putting closed the contrary sequencing valve of putting after finishing, the unlatching sequencing valve of finding time is found time to adsorbent bed, the end pressure of finding time is about 0.025MPa, close the sequencing valve of finding time after finding time to finish, the vinyl chloride that content is about 98.5% (volume %) in contrary venting and the exhaust is as out-of-bounds recycling of vinyl chloride product gas output.Open shoulder and all press sequencing valve that adsorbent bed is communicated with the surge tank of all calming the anger to carry out equal voltage rise, close after all voltage rise is finished and all press sequencing valve, open shoulder pressurising sequencing valve utilization absorption waste gas and adsorbent bed is finally boosted to adsorptive pressure prepare to enter next working cycles.
Table 10 embodiment 5 pressure-swing absorption apparatus sequencing valve time-scales
| Divide the cycle | 1 | 2 | 3 | 4 | ||||||||||||
| The A tower | A | ED | RP | D | V | ER | FR | |||||||||
| The B tower | V | ER | FR | A | ED | RP | D | V | ||||||||
| The C tower | RP | D | V | ER | FR | A | ED | RP | ||||||||
| The D tower | ED | RP | D | V | ER | FR | A | |||||||||
Claims (4)
1, a kind of pressure swing absorption process that reclaims vinyl chloride that from the vinyl-chloride-containing gaseous mixture, concentrates, it is characterized in that at least two adsorbent bed systems, each adsorbent bed experiences absorption successively, at least once all pressure drops, displacement, contrary putting, find time, at least once all voltage rises or boost with displacement waste gas and to add at least once all voltage rise replacements, the step of finally boosting, by the contrary product gas of putting and find time to obtain to be rich in vinyl chloride, adsorbent bed is filled with active carbon, activated alumina, at least a adsorbent in the silica gel, adsorptive pressure is greater than 0.15MPa, pressure was 0.01MPa～0.06MPa when evacuation step was finished, displacement step pressure is 0.15MPa～1.0MPa, pressure is 0.1MPa～0.15MPa when finishing against putting, the pressure that finally boosts when finishing is identical with adsorptive pressure, and the unstripped gas temperature is 5 ℃～60 ℃.
2, pressure swing absorption process according to claim 1 is characterized in that the composition of adsorbent and weight % are as follows:
Activated alumina 0～100%
Silica gel 0～100%
Active carbon 0～60%
3, pressure swing absorption process according to claim 1 is characterized in that equal voltage rise, equal voltage drop step are respectively 1～5 time.
4, pressure swing absorption process according to claim 1 is characterized in that introducing the vinyl chloride product gas that accounts for vinyl chloride product gas long-pending 5%～80% and after pressurizeing adsorbent bed is replaced in displacement step.
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| CN 200410040544 CN1259120C (en) | 2004-08-27 | 2004-08-27 | Pressure-varying adsorption method for concentrating and recovering chlorethylene from chlorethylene containing gas mixture |
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| CN101758659B (en) * | 2009-12-31 | 2012-10-24 | 孙宗长 | Device for increasing concentration and decreasing emission of waste gas in printer |
| CN102921271B (en) * | 2012-11-07 | 2015-04-29 | 四川天一科技股份有限公司 | Improved process for recovering non-methane hydrocarbon in polyolefin tail gases by adsorption method |
| CN104941388B (en) * | 2013-12-23 | 2019-10-15 | 中国科学院成都有机化学有限公司 | A method of separation vinyl chloride and acetylene |
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