CN104845657A - Purification system and process for recycling residual light oil in shale oil dry distillation tail gas - Google Patents
Purification system and process for recycling residual light oil in shale oil dry distillation tail gas Download PDFInfo
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Abstract
The invention relates to a purification system and a process for recycling the residual light oil in the shale oil dry distillation tail gas and belongs to the chemical industry technical field. The purification system comprises more than two adsorption beds, a heating system, a cooling system and a light oil recovery system; every adsorption bed is filled with adsorbent; the dry distillation tail gas enters the bottom of every adsorption bed, the purified dry distillation gas is output from the top of every adsorption bed through the adsorption, step-down, heating, cold blowing and boosting process, and the adsorption process is stopped when the content of the light oil in the purified dry distillation gas is higher than a required value. The process comprises the steps of adsorption, step-down, heating, cold blowing, boosting, recovery and the like. According to the purification system and the process for recycling the residual light oil in the shale oil dry distillation tail gas, the purification, the temperature swing adsorption and the removal are performed on the light oil in the dry distillation tail gas by a dry method according to the characteristics of the light oil in the shale oil dry distillation tail gas and accordingly the light oil in the dry distillation tail gas can be completely purified and removed and the purification accuracy of the dry distillation tail gas can reach the mg level.
Description
Technical field
The present invention relates to a kind of recovery in shale oil gas from dry distillation tail and remain lightweight oil cleaning system and technique, belong to chemical technology field.
Background technology
Resinous shale is the Mineral resources that a kind of standing stock are very abundant, not only can extract oil fuel, can also refine out combustion gas and industrial chemicals, and byproduct can the product such as brickmaking, cement, glass, pottery.According to national oil shale resources evaluation result, China's oil shale resources are 7199.37 hundred million tons, and the reserves being converted to shale oil are 476.44 hundred million tons, for China's natural crude oil verifies 4.14 times of workable reserve.Therefore, resinous shale is rising potential substitute energy.
Through cracking chemical transformation, the petrologen in resinous shale can be converted to synthetic crude.Heating oil shale produces the shale oil of similar oil to specified temp distillation---a kind of non-traditional oil and inflammable oil shale gas (" shale gas " also can refer to the natural-gas that shale includes).Similar natural oil, is rich in alkane and aromatic hydrocarbons, but containing more olefin component, and containing the non-hydrocarbons component containing oxygen, nitrogen, sulphur etc.Shale oil properties, different because of various places resinous shale composition and the difference of hot-work condition.The hydrogen-to-carbon ratio of the shale oil that China Fushun, Maoming, U.S.'s green river are produced is higher, is suitable for processing and produces light-end products; But because its nitrogen content is higher, must be removed during processing refining, otherwise can oil quality be affected.In the shale oil that Estonia produces, the oxygenatedchemicals such as phenols is a lot, is suitable for processing Valuable Chemicals.Fushun, Maoming shale oil, through suitable processing and refining, can obtain qualified gasoline, kerosene, diesel oil, fuel wet goods oil product, also can obtain the chemical by-products such as paraffin, phenols, pyridines, naphthenic acid and refinery coke.The method of shale oil processing is substantially identical with the refining process of natural oil, comprises the processes such as rectifying, thermally splitting, petroleum coking, hydrofining.
Producing light-end products from shale oil, is the one that current artificial petroleum produces that in the method for qualifying liquid fluid fuel, cost is minimum.
At present, the processing technology that resinous shale produces shale oil is divided into ground retorting technique and in-situ retorting technology.Ground retorting technique refers to resinous shale through strip mining transformation or tunnel, down-hole Mining Transport to ground, and through crushing and screening to required granularity or lumpiness, then transfer in gas retort, generate shale oil, shale gas and shale semicockes through heating low-temperature pyrolysis.And in-situ retorting technology is still in laboratory development, not yet carry out large-scale commercial application.At present, ground retorting technique is the main approach extracting shale oil from resinous shale.
Fig. 1 is shown in the method technical process of more Fushun its treated oil shale of stove retorting technique of domestic current use.Destructive distillation oil gas reclaims shale oil Posterior circle by subcooling and uses.In Xinjiang enterprise plant running situation, gas from dry distillation tail also contains C after being reclaimed by cooling
5-C
9lightweight oil 7-20g/Nm
3, prior art can not extract this part lightweight oil effectively, if this part recovering of vaporized hydrocarbons will effectively be improved oil product yield.
Summary of the invention
The object of the invention is to the defect overcoming prior art, provide a kind of and reclaim residual lightweight oil cleaning system and technique in shale oil gas from dry distillation tail, can by lightweight oil efficient recovery residual in shale oil gas from dry distillation tail.
The present invention is achieved through the following technical solutions:
A kind of recovery in shale oil gas from dry distillation tail remains lightweight oil cleaning system, and described purification system includes the adsorption bed of more than 2, heating system, cooling system and recovering of vaporized hydrocarbons system; Filled with adsorbent in described adsorption bed; Gas from dry distillation tail enters bottom adsorption bed, and experience absorption, step-down, heating, cold blowing, boost process, export the carbonization gas after purification by adsorption bed top, when lightweight oil content is higher than required value in the carbonization gas after purifying, stops adsorption process.When in carbonization gas after purification, lightweight oil content is higher than required value, sorbent material is saturated, need stop absorption.
As preferably, described sorbent material is two or more in inert alumina, activated alumina, coke, silica gel and gac.
As preferably, described recovering of vaporized hydrocarbons system comprises regeneration vapour cooler, water-and-oil separator and collector.
As preferably, in the carbonization gas after described purification, lightweight oil content requirement value is 50mg/Nm
3.
Adopt above-mentioned purification system to reclaim a technique for residual lightweight oil in shale oil gas from dry distillation tail, described technique comprises the following steps:
(1) adsorb: the gas from dry distillation tail of oil-containing enters adsorption bed bottom adsorption bed, lightweight oil in gas from dry distillation tail is by the adsorbent in adsorption bed, adsorption bed top exports the gas from dry distillation tail after purification, when in the gas from dry distillation tail after purifying, lightweight oil content is greater than required value, stop the charging of gas from dry distillation tail, stop absorption;
(2), step-down: after adsorption step terminates, to adsorption bed step-down, rely on the pressure in adsorption bed, automatically the gas in adsorption bed is got rid of bottom adsorption bed;
(3), heat: pass into from adsorption bed top with the water vapor that temperature is 150 DEG C ~ 200 DEG C, 140 DEG C ~ 180 DEG C are heated to adsorption bed, the lightweight oil adsorbed in adsorption bed is all vaporized into regeneration steam, together bottom adsorption bed, take adsorption bed out of with water vapor, sorbent material is regenerated;
(4), cold blowing: cold blowing gas enters from adsorption bed top, is taken out of by the waste heat in adsorption bed, until reach the gas from dry distillation tail temperature before passing into adsorption bed;
(5), boosting: the gas from dry distillation tail after purification slowly by adsorption bed pressurising, until reach absorption service pressure, come into operation when waiting for absorption next time.
(6), reclaim: recovering of vaporized hydrocarbons system reclaims the regeneration steam that step (3) obtains; Regeneration steam obtains oil-water mixture after the cooling of regeneration steam condenser, is separated and obtains lightweight oil after oil-water mixture enters water-and-oil separator.
As preferably, the absorption operating pressure 0.005MPa.g ~ 1.0MPa.g of described step (1).
As preferably, the cold blowing gas of described step (4) is nitrogen.
As preferably, the gas from dry distillation tail pressure passing into adsorption bed is 0.005MPa.g ~ 1.0MPa.g, temperature is 20 DEG C ~ 40 DEG C, and flow is 1000-50000Nm
3/ h.
Often close adsorption bed and all experience identical step, just order is upper intersects mutually, to ensure that scavenging process carries out continuously, obtains the carbonization gas after stable purification.
Compared with prior art, the invention has the beneficial effects as follows: the lightweight oil characteristic that the present invention is directed to shale oil gas from dry distillation tail, adopt the lightweight oil in dry cleaning temperature swing adsorbing and removing gas from dry distillation tail, can purify the lightweight oil removed in gas from dry distillation tail completely, its purification precision can reach mg level level.
By removing the gas from dry distillation tail after lightweight oil, its lightweight oil content can reach l0mg/Nm
3following level, the lightweight oil of recovery meets shale oil product requirement and can effectively improve oil product yield.And the adsorption bed of this technique can regenerate, can reuse, thus running cost is low, simple to operate.
Figure of description
Fig. 1 is the process flow sheet of Fushun stove retorting technique treated oil shale;
Fig. 2 is process flow diagram of the present invention.
Embodiment
Below in conjunction with embodiment, foregoing invention content of the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacement and change, all should comprise within the scope of the invention.
A kind of reclaim residual lightweight oil cleaning system in shale oil gas from dry distillation tail, described purification system is the above purification system of one-level, and every grade of purification system includes the adsorption bed of more than 2, heating system, cooling system and recovering of vaporized hydrocarbons system; Filled with adsorbent in described adsorption bed; Gas from dry distillation tail enters bottom adsorption bed, experience absorption (A), step-down (D), heating (H), cold blowing (C), boosting (R) process, the carbonization gas after purification is exported, when in the carbonization gas after purification, lightweight oil content is greater than required value 50mg/Nm by adsorption bed top
3time, stop adsorption process.Sorbent material is two or more in inert alumina, activated alumina, coke, silica gel and gac, and recovering of vaporized hydrocarbons system comprises regeneration vapour cooler, water-and-oil separator and collector.
Adopt as above-mentioned purification system reclaims the technique remaining lightweight oil in shale oil gas from dry distillation tail, comprise the following steps:
(1) adsorb (A): pressure be 0.020MPa.g, temperature is 20 DEG C ~ 40 DEG C, flow is 5000Nm
3the oil-containing gas from dry distillation tail of/h enters adsorption bed bottom adsorption bed, lightweight oil in gas from dry distillation tail is by the adsorbent in adsorption bed, adsorption bed top exports the gas from dry distillation tail after purification, when in the gas from dry distillation tail after purifying, lightweight oil content is greater than required value, stop the charging of gas from dry distillation tail, stop absorption, absorption operating pressure 0.005MPa.g ~ 1.0MPa.g;
(2), step-down (D): after adsorption step terminates, to adsorption bed step-down, rely on the pressure in adsorption bed, automatically the gas in adsorption bed is got rid of bottom adsorption bed;
(3), (H) is heated: be that the water vapor of 150 ~ 200 DEG C passes into from adsorption bed top by temperature, 140 ~ 180 DEG C are heated to adsorption bed, the lightweight oil adsorbed in adsorption bed is all vaporized into regeneration steam, together bottom adsorption bed, take adsorption bed out of with water vapor, sorbent material is regenerated;
(4), cold blowing (C): nitrogen enters from adsorption bed top, is taken out of by the waste heat in adsorption bed, until reach the gas from dry distillation tail temperature before passing into adsorption bed;
(5), boosting (R): the gas from dry distillation tail after purification slowly by adsorption bed pressurising, until reach absorption service pressure, come into operation when waiting for absorption next time.
(6), reclaim: recovering of vaporized hydrocarbons system reclaims the regeneration steam that step (3) obtains; Regeneration steam obtains oil-water mixture after the cooling of regeneration steam condenser, is separated and obtains lightweight oil after oil-water mixture enters water-and-oil separator.
Often close adsorption bed and all experience identical step, just order is upper intersects mutually, to ensure that scavenging process carries out continuously, obtains the carbonization gas after stable purification.
Embodiment 1
The present embodiment is the lightweight oil that employing shale oil gas from dry distillation tail dry cleaning temperature swing adsorption process recycles in following gas from dry distillation tail:
The pressure of gas from dry distillation tail is for being 20 ~ 40 DEG C for 0.020MPa.g, temperature, and flow is 5000Nm
3/ h,
Gas from dry distillation tail is mainly composed as follows:
| Component | O 2 | N 2 | CH 4 | H 2 | CO | CO 2 | C 2H 4 | C 2H 6 | Lightweight oil |
| Content (V%) | 0.39 | 14.9 | 18.8 | 18 | 13.8 | 28.1 | 4.2 | 1.0 | 0.81 |
Wherein lightweight oil is mainly composed as follows:
| Component | C4 | C5 | C6 | C7 | C8 | C9 | C10 |
| Content (wt%) | 0.12 | 4.01 | 19.49 | 32.46 | 32.34 | 11.25 | 0.33 |
According to the requirement that lightweight oil in gas from dry distillation tail removes, its adsorbing and removing system adopts 4 adsorption bed technical process.
After absorption, the lightweight oil content in gas from dry distillation tail can reach≤requirement of 20mg/Nm3.
Specific embodiment is analysed as follows in detail:
In 4 adsorption bed technical process, have 2 adsorption beds to be in adsorption process, other 2 adsorption beds are in reproduced state simultaneously; Adsorption bed filling gac class sorbent material.The order that each adsorption bed runs is as shown in the table:
Every platform adsorption bed first carries out adsorbing (A) process, then carry out regenerative process, wait for (E) process, cold blowing (C) process and boosting (R) process comprising step-down (D) process, heating (H) process, isolation.Gas from dry distillation tail enters bottom adsorption bed, after removing lightweight oil, exports the carbonization gas after purification by adsorption bed top by adsorption bed; When lightweight oil content exceedes required value in the carbonization gas after purifying, stop adsorption process.Adsorption process pressure keeps the system pressure of 0.020MPa.g always.Adsorption process terminates adsorption bed and enters step-down (D) process, the pressure in adsorption bed is dropped to the equilibrium pressure of heat-processed.After adsorption bed pressure drops to thermal regeneration pressure, by steam heating to 150-170 DEG C, to adsorption bed internal adsorption agent heating, adsorbent temperature reaches more than 150 DEG C, maintains this temperature until impurity is all taken out of in adsorption bed, stops heating.Introduce nitrogen at room and carry out cold blowing cooling to sorbent material, until be less than 40 DEG C, cold blowing terminates.Adsorption bed is boosted to pressure 0.020MPa.g during absorption by the gas from dry distillation tail after cold blowing terminates rear purification, and boost process as far as possible slowly.The adsorption bed rising good pressure can drop into absorption at any time.
Adsorption bed is in thermal regeneration process and cold blowing process, lightweight oil takes adsorption bed out of with heating steam or cold blowing gas, this mixture is introduced regeneration vapour cooler, cool to about 40 DEG C, water, lightweight oil are condensed into liquid and enter water-and-oil separator, by water-and-oil separator, water of condensation is separated with lightweight oil, lightweight oil and recyclable.
Embodiment 2
The present embodiment is the lightweight oil that employing shale oil gas from dry distillation tail dry cleaning temperature swing adsorption process recycles in following gas from dry distillation tail:
The pressure of gas from dry distillation tail is for being 20 ~ 40 DEG C for 0.050MPa.g, temperature, and flow is 50000Nm
3/ h,
Gas from dry distillation tail is mainly composed as follows:
| Component | O 2 | N 2 | CH 4 | H 2 | CO | CO 2 | C 2H 4 | C 2H 6 | Lightweight oil |
| Content (V%) | 0.17 | 13.5 | 19.2 | 18.3 | 13.5 | 27.8 | 4.3 | 1.5 | 1.73 |
Wherein lightweight oil is mainly composed as follows:
| Component | C4 | C5 | C6 | C7 | C8 | C9 | C10 |
| Content (wt%) | 0.08 | 5.91 | 21.82 | 29.45 | 30.18 | 12.35 | 0.21 |
According to the requirement that lightweight oil in gas from dry distillation tail removes, its adsorbing and removing system adopts 7 adsorption bed technical process.
After absorption, the lightweight oil content in gas from dry distillation tail can reach≤requirement of 50mg/Nm3.
Specific embodiment is analysed as follows in detail:
In 7 adsorption bed technical process of adsorption system, have 6 adsorption beds to be in adsorption process, other 1 adsorption bed is in reproduced state simultaneously; Adsorption bed filling gac class sorbent material and alumina adsorbant.The order that each adsorption bed runs is as shown in the table:
Every platform adsorption bed first carries out adsorbing (A) process, then carries out regenerative process, comprising step-down (D) process, heating (H) process, cold blowing (C) process and boosting (R) process.Gas from dry distillation tail enters bottom adsorption bed, after removing lightweight oil, exports the carbonization gas after purification by adsorption bed top by adsorption bed; When lightweight oil content exceedes required value in the carbonization gas after purifying, stop adsorption process.Adsorption process pressure keeps the system pressure of 0.050MPa.g always.Adsorption process terminates adsorption bed and enters step-down (D) process, the pressure in adsorption bed is dropped to the equilibrium pressure of heat-processed.After adsorption bed pressure drops to thermal regeneration pressure, by steam heating to 144-160 DEG C, to adsorption bed internal adsorption agent heating, adsorbent temperature reaches more than 144 DEG C, maintains this temperature until impurity is all taken out of in adsorption bed, stops heating.Introduce nitrogen at room and carry out cold blowing cooling to sorbent material, until be less than 40 DEG C, cold blowing terminates.Adsorption bed is boosted to pressure 0.050MPa.g during absorption by the gas from dry distillation tail after cold blowing terminates rear purification, and boost process as far as possible slowly.The adsorption bed rising good pressure can drop into absorption at any time.
Adsorption bed is in thermal regeneration process and cold blowing process, lightweight oil takes adsorption bed out of with heating steam or cold blowing gas, this mixture is introduced regeneration steam condenser, cool to about 40 DEG C, water, lightweight oil are condensed into liquid and enter water-and-oil separator, by water-and-oil separator, water of condensation is separated with lightweight oil, lightweight oil and recyclable.
For embodiment 2, the present invention is adopted to reclaim the lightweight oil in gas from dry distillation tail, recyclable lightweight oil per hour about 3.8 tons, calculate by annual 8000 hours, 1 year recyclable lightweight oil about 30000 tons, by oil product price per ton 5000 yuan calculating, the lightweight oil that recoverable value is 1.5 hundred million yuans, this plant investment about 4,000 ten thousand yuan, go out manually and other running cost, the present invention can create considerable economic worth.
Claims (8)
1. reclaim a residual lightweight oil cleaning system in shale oil gas from dry distillation tail, it is characterized in that: described purification system includes the adsorption bed of more than 2, heating system, cooling system and recovering of vaporized hydrocarbons system; Filled with adsorbent in described adsorption bed; Gas from dry distillation tail enters bottom adsorption bed, and experience absorption, step-down, heating, cold blowing, boost process, export the carbonization gas after purification by adsorption bed top, when lightweight oil content is higher than required value in the carbonization gas after purifying, stops adsorption process.
2. residual lightweight oil cleaning system in recovery shale oil gas from dry distillation tail according to claim 1, is characterized in that: described sorbent material is two or more in inert alumina, activated alumina, coke, silica gel and gac.
3. residual lightweight oil cleaning system in recovery shale oil gas from dry distillation tail according to claim 1, is characterized in that: described recovering of vaporized hydrocarbons system comprises regeneration vapour cooler, water-and-oil separator and collector.
4. residual lightweight oil cleaning system in recovery shale oil gas from dry distillation tail according to claim 1, is characterized in that: in the carbonization gas after described purification, lightweight oil content requirement value is 50mg/Nm
3.
5. adopt purification system as described in any one of Claims 1-4 to reclaim a technique for residual lightweight oil in shale oil gas from dry distillation tail, it is characterized in that, described technique comprises the following steps:
(1) adsorb: the gas from dry distillation tail of oil-containing enters adsorption bed bottom adsorption bed, lightweight oil in gas from dry distillation tail is by the adsorbent in adsorption bed, adsorption bed top exports the gas from dry distillation tail after purification, when in the gas from dry distillation tail after purifying, lightweight oil content is greater than required value, stop the charging of gas from dry distillation tail, stop absorption;
(2), step-down: after adsorption step terminates, to adsorption bed step-down, rely on the pressure in adsorption bed, automatically the gas in adsorption bed is got rid of bottom adsorption bed;
(3), heat: pass into from adsorption bed top with the water vapor that temperature is 150 DEG C ~ 200 DEG C, 140 DEG C ~ 180 DEG C are heated to adsorption bed, the lightweight oil adsorbed in adsorption bed is all vaporized into regeneration steam, together bottom adsorption bed, take adsorption bed out of with water vapor, sorbent material is regenerated;
(4), cold blowing: cold blowing gas enters from adsorption bed top, is taken out of by the waste heat in adsorption bed, until reach the gas from dry distillation tail temperature before passing into adsorption bed;
(5), boosting: the gas from dry distillation tail after purification slowly by adsorption bed pressurising, until reach absorption service pressure, come into operation when waiting for absorption next time;
(6), reclaim: recovering of vaporized hydrocarbons system reclaims the regeneration steam that step (3) obtains; Regeneration steam obtains oil-water mixture after the cooling of regeneration steam condenser, is separated and obtains lightweight oil after oil-water mixture enters water-and-oil separator.
6. purification system according to claim 5 reclaims the technique of residual lightweight oil in shale oil gas from dry distillation tail, it is characterized in that: absorption operating pressure 0. 005 MPa.g ~ 1. 0MPa.g of described step (1).
7. purification system according to claim 5 reclaims the technique of residual lightweight oil in shale oil gas from dry distillation tail, it is characterized in that: the cold blowing gas of described step (4) is nitrogen.
8. purification system according to claim 5 reclaims the technique of residual lightweight oil in shale oil gas from dry distillation tail, it is characterized in that: the gas from dry distillation tail pressure passing into adsorption bed is 0. 005 MPa.g ~ 1. 0MPa.g, temperature is 20 DEG C ~ 40 DEG C, and flow is 1000-50000Nm
3/ h.
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| CN106621695A (en) * | 2016-11-21 | 2017-05-10 | 湖北绿色家园材料技术股份有限公司 | Method for treating and recycling tail gas produced during benzaldehyde production |
| CN107216923A (en) * | 2017-06-27 | 2017-09-29 | 成都深冷液化设备股份有限公司 | The composite bed adsorbent equipment of natural gas pretreatment |
| CN110302632A (en) * | 2019-06-14 | 2019-10-08 | 北京科技大学 | A kind of raw material gas purifying system and technique |
| CN113499663A (en) * | 2021-08-10 | 2021-10-15 | 西安瀚宇树脂科技有限公司 | Resource treatment and recovery method for shale oil dry distillation refining waste gas |
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| CN101323799A (en) * | 2008-07-29 | 2008-12-17 | 四川天一科技股份有限公司 | Coke oven gas dry cleaning temperature swing adsorption process |
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| CN204281681U (en) * | 2014-11-30 | 2015-04-22 | 东北电力大学 | A kind of retrieving arrangement of steam adsorption desorption oil shale distillation gas lightweight oil |
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| CN101323799A (en) * | 2008-07-29 | 2008-12-17 | 四川天一科技股份有限公司 | Coke oven gas dry cleaning temperature swing adsorption process |
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| CN106621695A (en) * | 2016-11-21 | 2017-05-10 | 湖北绿色家园材料技术股份有限公司 | Method for treating and recycling tail gas produced during benzaldehyde production |
| CN107216923A (en) * | 2017-06-27 | 2017-09-29 | 成都深冷液化设备股份有限公司 | The composite bed adsorbent equipment of natural gas pretreatment |
| CN110302632A (en) * | 2019-06-14 | 2019-10-08 | 北京科技大学 | A kind of raw material gas purifying system and technique |
| CN113499663A (en) * | 2021-08-10 | 2021-10-15 | 西安瀚宇树脂科技有限公司 | Resource treatment and recovery method for shale oil dry distillation refining waste gas |
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Application publication date: 20150819 |