CN1283755C - Pretreating method for diesel-fuel of poor quality - Google Patents
Pretreating method for diesel-fuel of poor quality Download PDFInfo
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- CN1283755C CN1283755C CN 200510017365 CN200510017365A CN1283755C CN 1283755 C CN1283755 C CN 1283755C CN 200510017365 CN200510017365 CN 200510017365 CN 200510017365 A CN200510017365 A CN 200510017365A CN 1283755 C CN1283755 C CN 1283755C
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Abstract
The present invention discloses a pretreating method for poor-quality diesel oil, which comprises the following steps: the raw material of poor-quality diesel oil is in contact with adsorbing agents to carry out adsorption filtration under the conditions that the adsorption temperature is from 50 to 150DEG. C and the air speed of the adsorption volume is from 1.0 to 5.0h<-1>; the adsorbing agents are in contact with desorbing agents to carry out desorption after the adsorbing agents are saturated by adsorption; the adsorbing agents are scorched and regenerated after the adsorbing agents are adsorbed and desorbed for many times; the adsorbing agents of which the polarity is recovered is repeatedly used. After the poor-quality diesel oil treated by the method of the present invention, the gelatine removal rate is from 50 to 70%, and the loss of the feeding oil product is smaller than 0.5 wt. %. The diesel oil pretreated by the present invention enables the operating period of a subsequent hydrogenation unit to be extended about one year.
Description
Technical field
The invention belongs to petrochemical industry, relate to a kind of pretreating method for diesel-fuel of poor quality.
Background technology
In recent years, the demand of diesel oil grows with each passing day on the market.The general light oil yield of crude oil in China is low, and secondary processing diesel oil such as catalytic diesel oil, coker gas oil proportion is very big in the diesel oil.It is heavy that crude oil becomes day by day, makes the quality of secondary processing diesel oil also become worse and worse, thereby can not meet the need of market.Along with the new environmental regulation in the continuous expansion of domestic heavy oil deep processing ability and the world to diesel quality require strict further, it is more outstanding that this problem seems, this is objectively also promoting the diesel oil hydrogenation technology rapid development.
In the hydrogenation process of secondary processing diesel oil, owing to contain a large amount of alkene in the raw material, aromatic hydrocarbons and the sulfide that can cause and promote polyreaction, nitride, therefore in the course of processing, can generate some macromole colloids inevitably, even generate insoluble oxidation sediment, these materials deposit in the heat-exchange system of hydrogenation process on the one hand, reduce the heat exchange efficiency of interchanger, on the other hand easily in the bed coking of hydrogenator top, influence reactor performance, reduce activity of hydrocatalyst, can cause improper shut-down when serious and shorten the running period of hydrogenation unit.
As everyone knows, the raw material filter method that present diesel hydrotreating unit generally adopts is the mechanical filter method, promptly adopt mechanical means such as strainer, filter to remove solid matters such as mechanical impurity in the raw material and sediment, but this method can not be removed the macromole colloid, and in the work-ing life of stopping up filter screen easily and reducing filter plant, the problem of hydrogenator top bed coking is also unresolved simultaneously.
Up to now, yet there are no and adopt sorbent material that the raw material of diesel hydrotreating unit is carried out pretreated report.
Summary of the invention
The present invention can not remove macromole colloid in the diesel raw material for overcoming the method for handling raw material in the existing diesel hydrotreating unit, and the work-ing life of stopping up filter screen easily and reducing filter plant, and propose a kind ofly can remove solid matters such as mechanical impurity in the raw material and sediment, can remove macromole gelationus poor ignition quality fuel pre-treatment novel method again.
Pretreating method for diesel-fuel of poor quality provided by the invention, its step comprises: the poor ignition quality fuel raw material is 50～150 ℃ at adsorption temp, the adsorption volume air speed is 1.0～5.0h
-1Condition under, contact with sorbent material and to carry out adsorption filtration, the saturated back of adsorbents adsorb contacts with desorbing agent carries out desorption, and desorption temperature is 100～200 ℃, and the weight ratio of desorbing agent and sorbent material is 0.10～0.13, desorption time is 2～6h, repeat the adsorption/desorption process, to adsorbents adsorb saturated after, with thermal barrier sorbent material is carried out coke burning regeneration, the coke burning regeneration temperature is 300～450 ℃, recovers the polar sorbent material and reuses.Described sorbent material is a kind of in impregnated silicon-dioxide, titanium oxide, zeolite, aluminum oxide, diatomite and pure aluminium silicate etc., impregnation of matters is selected from phosphoric acid, alkali-metal oxyhydroxide or alkali-metal salt, impregnation of matters behind dipping in the sorbent material shared weight percentage be 10～50%, described thermal barrier is the indifferent gas (as stack gas or nitrogen etc.) that contains oxygen.
Desorbing agent described in the inventive method is conventional indifferent gas, as stack gas, nitrogen or water vapour etc.
The coke burning regeneration of sorbent material of the present invention can carry out in-situ regeneration or device is regenerated outward according to common coke burning regeneration method, and the outer regenerated advantage of device is an easy handling, and solid matter is sieved remove easily.When adsorbent reactivation process of the present invention adopted in-situ regeneration, the oxygen level in the indifferent gas was 1～3 volume %; When adopting device to regenerate outward, oxygen level 1～10 volume % in the indifferent gas.
The method of sorbent material in-situ regeneration of the present invention is, the indifferent gas (as stack gas or nitrogen etc.) that feeds oxygen level 1～3 volume % in adsorption tower carries out coke burning regeneration in the device to sorbent material, regulate the thermal barrier oxygen level according to the adsorption tower temperature in, the coke burning regeneration temperature is 300～450 ℃, recovery time 4～12h, this moment, the polarity recovery rate of sorbent material was not less than 97%.The outer regenerated method of device is, sorbent material is drawn off, adopt two travelling belts, fix the sorbent material of many pallets on each travelling belt with carrying thickness 2～5cm, on first travelling belt, sorbent material contacts 1～4h with the indifferent gas of 300～350 ℃ oxygen level 1～10 volume %, to remove the oil content in the sorbent material, deliver to second travelling belt afterwards, contact 4～12h at 400～450 ℃ of indifferent gas and carry out coke burning regeneration with oxygen level 1～10 volume %, according to recovery time and regeneration temperature adjusting thermal barrier oxygen level, regeneration back sorbent material polarity recovery rate is not less than 97%.
Pretreating method for diesel-fuel of poor quality provided by the invention can adopt the mode that down-flow fixed bed adsorption tower, multitower switch that diesel raw material is carried out adsorption filtration, and the adsorption volume air speed of this moment is 1.0～5.0h
-1When adopting two towers to carry out blocked operation, diesel oil enters an adsorption tower from top, filter by sorbent material, when the sorbent material of this tower reaches certain absorption saturation ratio, diesel oil switches in second adsorption tower and carries out adsorption filtration, this moment, first adsorption tower entered the desorption stage, and is stand-by behind the desorption.When second adsorption tower reached certain absorption saturation ratio, diesel oil switched in first adsorption tower behind the desorption, and second adsorption tower enters the desorption stage.When sorbent circulation is used repeatedly, after general 8～12 times, solid matters such as the macromole colloid of its inner absorption and the mechanical impurity of surface deposition and sediment can get more and more, its polarity also reduces gradually, need carry out coke burning regeneration to recover sorbent material polarity, this moment, first adsorption tower entered the regeneration stage, and the regeneration back is stand-by; When second adsorption tower regenerated, diesel oil switched to first adsorption tower after the regeneration.So the circulation blocked operation reaches the purpose to the diesel oil adsorption filtration.
The present invention is applicable to the pre-treatment of poor ignition quality fuel, is mainly used in the filtration of diesel oil hydrogenation process raw material, also can be used for the filtration or the pre-treatment of other distillate hydrogenation device raw material.
Poor ignition quality fuel after adsorption filtration method of the present invention is handled, colloid decreasing ratio 50～70%, charging oil product loss＜0.5 weight %, sorbent material polarity recovery rate is not less than 97%.Use method provided by the invention not only can remove solid matters such as mechanical impurity and sediment, and can remove the macromole colloid, make actual gum content significantly reduce, can remove simultaneously part or impurity such as most of sulphur, nitrogen, its quality is significantly improved, charging as hydrogenation unit can obviously reduce the coking of reactor head bed, and make the hydrogenation catalyst initial reaction temperature reduce by 5～10 ℃, by 0.03～0.05 ℃/d of average temperature rising, hydrogenation unit is improved about 1 year running period.
The adsorption filtration method of diesel oil hydrogenation process raw material of the present invention mainly contains following advantage:
1. impurity removal percentage height can significantly improve the quality of charging.
2. filter plant is simple, and material is not had particular requirement, invests lower.
3. the filtration process method is simple, easily operation.
4. the sorbent material raw material is easy to get, and the preparation method is simple, and renewable recycling.
5. can obviously reduce the bed coking of hydrogenator top, device is improved about 1 year running period.
Embodiment
The present invention will be described in detail with specific embodiment below, but do not limit the scope of the invention.
Embodiment 1:
It is 40w% that analytical pure phosphoric acid is become concentration with distilled water diluting, and this solution 375ml is dipped on the 350g aluminum oxide, and handled 4 hours at 150 ℃ dry back, is modulated into the sorbent material of phosphorus acid content 30w%.This sorbent material 200ml is packed in the adsorption column of φ 20mm, the catalytic cracking diesel oil (raw material A) of sulphur content 5868 μ g/g, nitrogen content 1256 μ g/g, actual gum content 435mg/100ml is added in the tubualted bottle, take the drip mode to inject adsorption column from top, pass through the adsorbent bed adsorption filtration of carrying out, stop charging behind the 8h, carry out desorption from the stack gas that the bottom feeds after heating, stop air inlet behind the 4h, continue absorption from the top oil-feed.After so cyclical operation 10 is taken turns, stop charging, feed the stack gas of oxygen level 2v% then, keep 450 ℃ of bed temperatures, regeneration 6h continues charging afterwards, repeats aforesaid operations.Feed impurities content is referring to table 1～2 before and after raw material A processing condition, the filtration.
Table 1 raw material A processing condition
| Project | Parameter value |
| Adsorption temp, ℃ | 80 |
| The adsorption volume air speed, h -1 | 2.0 |
| Adsorption time, h | 8 |
| Desorption temperature, ℃ | 120 |
| Desorption gas agent ratio, w/w | 0.13 |
| Desorption time, h | 4 |
| The coke burning regeneration temperature, ℃ | 450 |
| Recovery time, h | 6 |
Feed impurities content before and after table 2 raw material A is filtered
| Project | Before the filtration | After the filtration | |
| Fresh adsorbent | Reproducing adsorbent | ||
| Feed impurities content | |||
| Sulphur, μ g/g | 5868 | 4776 | 4800 |
| Nitrogen, μ g/g | 1256 | 776 | 785 |
| Existent gum, mg/100ml | 435 | 177 | 183 |
| The adsorption filtration effect | |||
| Desulfurization degree, % | 18.6 | 18.2 | |
| Denitrification percent, % | 38.2 | 37.5 | |
| The colloid decreasing ratio, % | 59.3 | 58.0 | |
| The charging loss, w% | 0.33 | 0.31 | |
| Sorbent material polarity recovery rate, % | 97.5 | ||
By table 1 and table 2 as can be seen, at 80 ℃ of adsorption temps, adsorption volume air speed 2.0h
-1, under the adsorption time 8h, 120 ℃ of desorption temperatures, the processing condition of desorption gas agent than (w/w) 0.13, desorption time 4h, desulfurization degree 18.6%, denitrification percent 38.2%, colloid decreasing ratio 59.3%, charging loss 0.33w%; Sorbent material polarity recovery rate 97.5% under 450 ℃ of conditions of coke burning regeneration temperature.
Embodiment 2:
It is 30w% that analytical pure Repone K is become concentration with distilled water diluting, and this solution 500ml is dipped on the 600g pure aluminium silicate, and handled 4 hours at 200 ℃ dry back, is modulated into the sorbent material of KCE content 20w%.This sorbent material 200ml is packed in the adsorption column of φ 20mm, the coker gas oil (raw material B) of sulphur content 7646 μ g/g, nitrogen content 1024 μ g/g, actual gum content 257mg/100ml is added in the tubualted bottle, take the drip mode to inject adsorption column from top, pass through the adsorbent bed adsorption filtration of carrying out, stop charging behind the 10h, carry out desorption from the stack gas that the bottom feeds after heating, stop air inlet behind the 6h, continue absorption from the top oil-feed.After so cyclical operation 8 is taken turns, stop charging, draw off sorbent material then, adopt the stack gas of oxygen level 5v% that it is carried out device and regenerate outward, the 8h that regenerates under 430 ℃ of temperature, the sorbent material after will the regenerate afterwards adsorption column of packing into continues charging, the repetition aforesaid operations.Feed impurities content is referring to table 3～4 before and after raw material B processing condition, the filtration.
As can be seen, at 110 ℃ of adsorption temps, adsorption volume air speed 3.0h
-1, under the adsorption time 10h, 150 ℃ of desorption temperatures, the processing condition of desorption gas agent than (w/w) 0.11, desorption time 6h, desulfurization degree 55.2%, denitrification percent 37.6%, colloid decreasing ratio 65.8%, charging loss 0.42w%; Sorbent material polarity recovery rate 99.2% behind 430 ℃ of coke burning regenerations.
Table 3 raw material B processing condition
| Project | Parameter value |
| Adsorption temp, ℃ | 110 |
| The adsorption volume air speed, h -1 | 3.0 |
| Adsorption time, h | 10 |
| Desorption temperature, ℃ | 150 |
| Desorption gas agent ratio, w/w | 0.11 |
| Desorption time, h | 6 |
| The coke burning regeneration temperature, ℃ | 430 |
| Recovery time, h | 8 |
Feed impurities content before and after table 4 raw material B filters
| Project | Before the filtration | After the filtration | |
| Fresh adsorbent | Reproducing adsorbent | ||
| Feed impurities content | |||
| Sulphur, μ g/g | 7646 | 3425 | 3456 |
| Nitrogen, μ g/g | 1024 | 639 | 642 |
| Existent gum, mg/100ml | 257 | 88 | 89 |
| The adsorption filtration effect | |||
| Desulfurization degree, % | 55.2 | 54.8 | |
| Denitrification percent, % | 37.6 | 37.3 | |
| The colloid decreasing ratio, % | 65.8 | 65.3 | |
| The charging loss, w% | 0.42 | 0.41 | |
| Sorbent material polarity recovery rate, % | 99.2 | ||
Embodiment 3:
It is 25w% that analytical pure sodium hydroxide is become concentration with distilled water diluting, and this solution 800ml is dipped on the 300g titanium oxide, and handled 4 hours at 180 ℃ dry back, is modulated into the sorbent material of sodium hydrate content 40w%.This sorbent material 200ml is packed in the adsorption column of φ 20mm, the thermally splitting diesel oil (raw material C) of sulphur content 5465 μ g/g, nitrogen content 1312 μ g/g, actual gum content 352mg/100ml is added in the tubualted bottle, take the drip mode to inject adsorption column from top, pass through the adsorbent bed adsorption filtration of carrying out, stop charging behind the 6h, carry out desorption from the stack gas that the bottom feeds after heating, stop air inlet behind the 3h, continue absorption from the top oil-feed.After so cyclical operation 12 is taken turns, stop charging, draw off sorbent material then, adopt the stack gas of oxygen level 7v% that it is carried out device and regenerate outward, the 10h that regenerates under 420 ℃ of temperature, the sorbent material after will the regenerate afterwards adsorption column of packing into continues charging, the repetition aforesaid operations.Feed impurities content is referring to table 5～6 before and after raw material C processing condition, the filtration.
As can be seen, at 130 ℃ of adsorption temps, adsorption volume air speed 4.0h
-1, under the adsorption time 6h, 180 ℃ of desorption temperatures, the processing condition of desorption gas agent than (w/w) 0.12, desorption time 3h, desulfurization degree 61.5%, denitrification percent 41.2%, colloid decreasing ratio 67.3%, charging loss 0.46w%; Sorbent material polarity recovery rate 97.8% behind 420 ℃ of coke burning regenerations.
Table 5 raw material C processing condition
| Project | Parameter value |
| Adsorption temp, ℃ | 130 |
| The adsorption volume air speed, h -1 | 4.0 |
| Adsorption time, h | 6 |
| Desorption temperature, ℃ | 180 |
| Desorption gas agent ratio, w/w | 0.12 |
| Desorption time, h | 3 |
| The coke burning regeneration temperature, ℃ | 420 |
| Recovery time, h | 10 |
Feed impurities content before and after table 6 raw material C filters
| Project | Before the filtration | After the filtration | |
| Fresh adsorbent | Reproducing adsorbent | ||
| Feed impurities content | |||
| Sulphur, μ g/g | 5465 | 2104 | 2181 |
| Nitrogen, μ g/g | 1312 | 771 | 783 |
| Existent gum, mg/100ml | 352 | 115 | 120 |
| The adsorption filtration effect | |||
| Desulfurization degree, % | 61.5 | 60.1 | |
| Denitrification percent, % | 41.2 | 40.3 | |
| The colloid decreasing ratio, % | 67.3 | 65.8 | |
| The charging loss, w% | 0.46 | 0.44 | |
| Sorbent material polarity recovery rate, % | 97.8 | ||
Embodiment 4:
To be raw material, adopt W-Ni/Al through embodiment 1 pretreated diesel oil
2O
3Hydrobon catalyst has carried out the 2000h investigation on medium-sized fixed bed hydrogenation testing apparatus, and contrasts with the mechanical filter method.Variation of hydrogenation catalyst average reaction temperature and top bed layer coke content are referring to table 7.
As can be seen from Table 7, compare with the mechanical filter method, adopt the adsorption filtration method can obviously reduce the coking of reactor head bed, 2000h does not have obvious temperature rise, and the hydrogenation catalyst initial reaction temperature reduces by 6～7 ℃, and hydrogenation unit is prolonged about 200 days running period.
Table 7 raw material A is filtered the back end hydrogenation catalyst reaction temperatures and is changed and top bed layer coke content
| Project | The hydrogenation catalyst average reaction temperature, ℃ | 2000h post-reactor top bed layer coke content, w% | |
| 50h | 2000h | ||
| The mechanical filter method | 321.0 | 326.5 | 6.6 |
| The adsorption filtration method | |||
| Fresh adsorbent | 314.0 | 315.3 | 1.8 |
| Reproducing adsorbent | 314.5 | 316.0 | 2.1 |
Embodiment 5:
To be raw material, adopt Co-Mo/Al through embodiment 2 pretreated diesel oil
2O
3Hydrobon catalyst has carried out the 2000h investigation on medium-sized fixed bed hydrogenation testing apparatus, and contrasts with the mechanical filter method.Variation of hydrogenation catalyst average reaction temperature and top bed layer coke content are referring to table 8.
As can be seen from Table 8, compare with the mechanical filter method, adopt the adsorption filtration method can obviously reduce the coking of reactor head bed, 2000h does not have obvious temperature rise, and the hydrogenation catalyst initial reaction temperature reduces by 9～10 ℃, can make hydrogenation unit prolong more than 300 day running period.
Table 8 raw material B filters the back end hydrogenation catalyst reaction temperatures to be changed and top bed layer coke content
| Project | The hydrogenation catalyst average reaction temperature, ℃ | 2000h post-reactor top bed layer coke content, w% | |
| 50h | 2000h | ||
| The mechanical filter method | 318.0 | 323.0 | 5.8 |
| The adsorption filtration method | |||
| Fresh adsorbent | 308.0 | 309.1 | 1.4 |
| Reproducing adsorbent | 308.4 | 309.7 | 1.7 |
Embodiment 6:
To be raw material, adopt W-Mo-Ni/Al through embodiment 3 pretreated diesel oil
2O
3Hydrobon catalyst has carried out the 2000h investigation on medium-sized fixed bed hydrogenation testing apparatus, and contrasts with the mechanical filter method.Variation of hydrogenation catalyst average reaction temperature and top bed layer coke content are referring to table 9.
As can be seen from Table 9, compare with the mechanical filter method, adopt the adsorption filtration method can obviously reduce the coking of reactor head bed, 2000h does not have obvious temperature rise, and the hydrogenation catalyst initial reaction temperature reduces by 10 ℃, can make hydrogenation unit prolong 1 year running period.
Table 9 raw material C filters the back end hydrogenation catalyst reaction temperatures to be changed and top bed layer coke content
| Project | The hydrogenation catalyst average reaction temperature, ℃ | 2000h post-reactor top bed layer coke content, w% | |
| 50h | 2000h | ||
| The mechanical filter method | 316.0 | 320.3 | 5.5 |
| The adsorption filtration method | |||
| Fresh adsorbent | 305.5 | 306.6 | 1.1 |
| Reproducing adsorbent | 306.2 | 307.5 | 1.4 |
Claims (3)
1. pretreating method for diesel-fuel of poor quality, it is characterized in that: the poor ignition quality fuel raw material is 50～150 ℃ at adsorption temp, the adsorption volume air speed is 1.0～5.0h
-1Condition under, contact with sorbent material and to carry out adsorption filtration, obtain pretreated diesel oil after the adsorption filtration, the saturated back of described adsorbents adsorb contacts with desorbing agent carries out desorption, desorption temperature is 100～200 ℃, the weight ratio of desorbing agent and sorbent material is 0.10～0.13, desorption time is 2～6h, repeat the adsorption/desorption process, to adsorbents adsorb saturated after, with thermal barrier sorbent material is carried out coke burning regeneration, the coke burning regeneration temperature is 300～450 ℃, recovers the polar sorbent material and reuses, described thermal barrier is the indifferent gas that contains oxygen, sorbent material is through impregnated silicon-dioxide, titanium oxide, zeolite, aluminum oxide, a kind of in diatomite and the pure aluminium silicate, impregnation of matters is selected from phosphoric acid, alkali-metal oxyhydroxide or alkali-metal salt, impregnation of matters behind dipping in the sorbent material shared weight percentage be 10～50%.
2. method according to claim 1 is characterized in that: described coke burning regeneration adopts in-situ regeneration, and the oxygen level in the indifferent gas is 1～3 volume %.
3. method according to claim 1 is characterized in that: described coke burning regeneration adopts device to regenerate outward, and the oxygen level in the indifferent gas is 1～10 volume %.
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| CN 200510017365 CN1283755C (en) | 2005-02-17 | 2005-02-17 | Pretreating method for diesel-fuel of poor quality |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102485845B (en) * | 2010-12-03 | 2014-01-15 | 中国石油天然气股份有限公司 | A method for denitrification and hydrogenation of secondary processed diesel oil |
| CN102660326A (en) * | 2012-05-31 | 2012-09-12 | 中国石油化工股份有限公司 | Hydroprocessing method of cracking C9 |
| CN104549131A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Adsorption desulfurization additive, as well as preparation method and desulfurization system thereof |
| CN104560123B (en) * | 2013-10-29 | 2016-08-24 | 中国石油化工股份有限公司 | A kind of method adsorbing desulfurization |
| CN106701171B (en) * | 2015-11-16 | 2019-05-03 | 神华集团有限责任公司 | A kind of processing method containing phenol oil in coal tar and a kind of processing method of coal tar |
| CN105368482B (en) * | 2015-12-11 | 2017-07-28 | 中海油天津化工研究设计院有限公司 | The method of polycyclic aromatic hydrocarbon in a kind of multitower adsorbing and removing diesel oil in parallel |
| CN108998090B (en) * | 2018-09-25 | 2021-06-15 | 浙江绿保再生资源科技有限公司 | Method for recycling waste oil |
| CN111534328A (en) * | 2020-05-12 | 2020-08-14 | 武汉科林化工集团有限公司 | Inferior high-olefin cracking carbon nine-fraction hydrogenation process |
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