CN1600837A - Steady hydrogenation method in counter current of oil liquefied from coal - Google Patents
Steady hydrogenation method in counter current of oil liquefied from coal Download PDFInfo
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- CN1600837A CN1600837A CN 03126443 CN03126443A CN1600837A CN 1600837 A CN1600837 A CN 1600837A CN 03126443 CN03126443 CN 03126443 CN 03126443 A CN03126443 A CN 03126443A CN 1600837 A CN1600837 A CN 1600837A
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Abstract
This invention provides a method of stable hydrogenation of coal-liquified oil by counter-current. It is characterized by that: coal-liquefied oil, after being filtered, is fed into the top of the reactor, while the hydrogen into the bottom of it, contacting with a hydrogenation protecting agent, a hydrogenation refining catalyst. The effluent from the stable hydrogenation reactor is proceeded via separation of high pressure separator, low pressure separator, fractional tower to obtain light wt. fractions and tail oil fractions. The gas flow rich in hydrogen from the high pressure separator is mixed with hydrogen and then circuled-back to the stable hydrogenation reactor. This invention method is of counter-current operation, so having advantages of: thorough liquid/gas contact, even temp. distribution in the reactor, improved reaction atmosphere, increased utilization rate of catalyst.
Description
Technical field
The present invention relates to the method that a kind of liquid hydrocarbon that coal destruction hydrogenation is obtained carries out hydrotreatment.More particularly, be a kind of liquefied coal coil hydrofinishing process.
Background technology
At present, coal and oil are main primary energy source, along with the development of Chinese national economy, to the demand of primary energy source in sustainable growth.Because the reinforcement of environmental consciousness, when the primary energy source demand increased, its consumption structure was also changing, coal in 1996 and oil account for that primary energy source consumes more than 92%, its PetroChina Company Limited. accounts for 17.5%, coal accounts for 75%; 1999, coal and oil accounted for 90.5% of China's primary energy source consumption, and its PetroChina Company Limited. accounts for 23.4%, and coal accounts for 67.1%.As seen, the ratio of China's primary energy source consumption PetroChina Company Limited. is progressively increasing.On the other hand, the rich coal resources of China and petroleum resources relative shortage, the import volume of oil is increasing year by year.Therefore, making full use of the coal resources of China's abundant, is liquid fuel by Technology of direct coal liquefaction with coal conversion, and to solving oil shortage, reduction national economy has great strategic importance to the dependency of Imported oil.
The history of the existing last 100 years of coal liquefaction, just having begun DCL/Direct coal liquefaction produced the liquid hydrocarbon product Study on Technology as far back as 1913 in Germany, and will make the skilled industryization of gasoline with the brown coal direct liquefaction in nineteen twenty-seven.Since the world oil crisis first time took place in 1973 since; direct coal liquefaction technology is subjected to the attention of developed country; developed many DCL/Direct coal liquefaction technologies in succession, wherein more representational technology is the HTI technology of U.S.'s exploitation, the IGOR technology of Germany's exploitation and the NEDOL technology of Japan's exploitation.
The key of gelatin liquefaction technology comprises the hydrotreatment part of liquefaction part and liquefaction oil.The main effect of liquefaction part is that solid-state coal is converted into liquid hydrocarbon, and the hydrotreatment part can comprise the impurity that removes in the liquefaction oil, improves its stable stable hydrogenation and further improve the hydro-upgrading of liquefaction oil quality.Wherein, stable hydrogenation can be cascaded with the liquefaction part, is called online stable hydrogenation, also can independently carry out, and is called the off-line stable hydrogenation.Aspect the stable hydrogenation of liquefied coal coil, HTI technology and IGOR process using online method of hydrotreating liquefied coal coil is carried out the first step hydrofining, be the gelatin liquefaction part producing hydrogen supply agent of front on the one hand, remove the heteroatoms in the product on the other hand as far as possible, reduce its alkene and aromaticity content, improve product stability.NEDOL process using off-line stable hydrogenation process carries out shallow degree hydrogenation with the liquefied coal coil that is used as hydrogen supply agent, and the processing of product upgrading is finished by subsequent technique.TOP NEDOL technology also adopts the method for off-line stable hydrogenation, but liquefied coal coil all advances hydrogenation unit, cuts out hydrogen supply agent from the hydrogenation after product.Their research thinking all is to utilize existing petroleum fractions hydrogenation catalyst (Mo/Ni or Mo/Co type carried catalyst) by optimizing hydrogenation conditions, draws hydrorefined operational path of the liquefied coal coil the first step and the condition of being suitable for.
US6190542B1 discloses a kind of technology of online hydrofining liquefied coal coil.The charging of the online hydrogenation unit of fixed bed is petroleum naphtha and diesel oil distillate or the full cut of liquefied coal coil, reaches the heteroatoms that removes in the liquefied coal coil by online hydrogenation, improves the purpose of liquefied coal coil stability, is gelatin liquefaction part producing hydrogen supply agent simultaneously.
US5332489 discloses a kind of method with hydrocracking process reconstructed coal liquefaction oil, and this technology is with the hydrogen supply agent of partial hydrogenation crackate as the gelatin liquefaction part, and all the other products go out coal liquification device as the product of coal liquification device.
Liquefied coal coil is identical at the flow direction of reactor with hydrogen in the above-mentioned prior art, promptly flows to the bottom from reactor top, and gas-to-liquid contact is insufficient, the reactor temperature skewness.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of liquefied coal coil adverse current stable hydrogenation process.
Method provided by the invention comprises: liquefied coal coil after the filtration and hydrogen enter the stable hydrogenation reactor from the upper and lower of reactor respectively, contact with hydrogenation protecting agent, Hydrobon catalyst, the stable hydrogenation reactor effluent passes through high-pressure separator, light pressure separator, separation column successively, separates to obtain lighting end and tail oil cut; Mix with fresh hydrogen from the isolated hydrogen rich stream of high-pressure separator, loop back the stable hydrogenation reactor.
The present invention adopts the stable hydrogenation of off-line to liquefied coal coil, the stable hydrogenation reactor adopts the operating method of reverse flow, gas-to-liquid contact is abundant, reactor temperature is evenly distributed, improved reaction atmosphere, the utilising efficiency of catalyzer is improved, and can be implemented in the hydrodenitrification of liquefied coal coil under the relative mitigation reaction conditions.
Description of drawings
Accompanying drawing is a liquefied coal coil adverse current stable hydrogenation process synoptic diagram provided by the invention.
Embodiment
Liquefied coal coil adverse current stable hydrogenation process operational path provided by the invention is as follows:
The liquefied coal coil that comes out from the gelatin liquefaction unit takes the measure of starvation to be transported to the stock oil surge tank, install after filtration in the filtering and removing liquefied coal coil behind the entrained solid particle, mix with the part circulating hydrogen after boosting to reaction pressure by feedstock pump, the effect of this part circulating hydrogen mainly is to prevent the pipeline coking.If guard reactor is set, then liquefied coal coil is introduced into guard reactor and contacts with the hydrogenation protecting agent, and the effusive logistics of guard reactor enters this reactor from stable hydrogenation reactor top, contacts with Hydrobon catalyst; Adopt the protection bed if guard reactor is not set, then liquefied coal coil earlier with the hydrogen mixing again with directly enter this reactor after the hydrogenation protecting agent contacts from stable hydrogenation reactor top, contact with Hydrobon catalyst; Circulating hydrogen enters from the stable hydrogenation reactor lower part, and liquefaction oil and hydrogen carry out hydrogenation reaction in the stable hydrogenation reactor, and stable hydrogenation reactor lower part effluent is the treated oil after the hydrotreatment, and hydrogen flows out from reactor top; The effusive treated oil in stable hydrogenation main reactor bottom enters separation system after heat exchange, the order that treated oil enters separation system is high-pressure separator, light pressure separator, separation column; By separation system isolate naphtha fraction, diesel oil distillate and＞370 ℃ tail oil cut; After washing, enter circulating hydrogen compressor from the effusive hydrogen in reactor top, the isolated hydrogen rich stream of high-pressure separator with wash after hydrogen together enter circulating hydrogen compressor after mixing, use as circulating hydrogen.
Raw material of the present invention is that boiling range is at C
5～500 ℃ liquefied coal coil, nitrogen content is not more than 2.0wt% in the raw material, and sulphur content is not more than 1.0wt%.The general three-phase fluidized bed that uses is as reactor in the gelatin liquefaction unit, and the used liquefied coal coil raw material of the present invention is exactly a three-phase fluidized bed liquid phase effluent, but does not comprise its contained solid phase.Owing to contain a large amount of alkene, nitrogen content height in the liquefied coal coil, generally more than 0.5m%, also contain a certain amount of oxygen, if untimelyly carry out pre-treatment, very easily generation is unfavorable for subsequent transportation and substances processed, therefore will adopt the method for hydrogenation liquefied coal coil to be carried out pre-treatment, the alkene in the saturated liquefied coal coil, maximum possible remove heteroatomss such as nitrogen, oxygen and sulphur, improve the stability of liquefied coal coil.
Owing to carry a large amount of solid particulate matters in the liquefied coal coil, therefore the present invention adds multistage automatic back-flushing filtering device before the hydro-refining unit feedstock pump, purpose is to filter out the solid particulate matter that carries in the liquefied coal coil, prevent reactor bed obstruction and the too fast inactivation of hydrogenation catalyst, improve the stability of device running and the life-span of hydrogenation catalyst.
The reaction conditions of liquefied coal coil stable hydrogenation technology of the present invention is: hydrogen dividing potential drop 3.0～30.0MPa; 270～450 ℃ of temperature of reaction; Liquid hourly space velocity 0.1～10h
-1, hydrogen-oil ratio 300～2800v/v.
The hydrogenation protecting agent of filling is VIB or VIII family non-precious metal catalyst or their combination that loads on unformed aluminum oxide or the silica-alumina supports in guard reactor or the protection bed.This type of protective material has bigger pore volume and specific surface area.
Described Hydrobon catalyst can be VIB or the VIII family non-precious metal catalyst that loads on unformed aluminum oxide or the silica-alumina supports, has very strong hydrodenitrogenationactivity activity.
In the guard reactor or the protective material loadings in the protection bed determine that itself and hydrofining agent volume ratio are 0.03～0.35 running period by foreign matter content in the liquefied coal coil and device.
Because liquefied coal coil was as hydrogen supply agent after most of coal liquefaction crafts needed a certain amount of hydrogenation, the technology that has will be as the independent hydrogenation of the liquefied coal coil of hydrogen supply agent, and all the other liquefied coal coils go out coal liquification device as product, the technology that has is with the whole hydrofinings of liquefied coal coil, improve stability, produce hydrogen supply agent simultaneously.The present invention carries out stable hydrogenation with whole liquefied coal coils and handles, and heavier part is as the hydrogen supply agent of gelatin liquefaction part.
If as the stable hydrogenation raw material, stable hydrogenation is divided into online again and the off-line dual mode with whole liquefied coal coils.Online hydrogenation unit and gelatin liquefaction partial common one cover hydrogen-feeding system, liquefied coal coil directly advances the stable hydrogenation device without surge tank.The off-line hydrogenation is exactly that the stable hydrogenation device has oneself independently hydrogen source and hydrogen gas circulating system, and the advanced raw material surge tank of liquefied coal coil advances the stable hydrogenation device again.
The present invention adopts the method for off-line that liquefied coal coil is carried out stable hydrogenation, adopts the off-line hydrogenation can avoid being rich in the liquefied coal coil influence of water vapour to hydrogenation catalyst, CO in the upstream gelatin liquefaction part gas phase
xCan not enter the stable hydrogenation device, reduce by CO
xHydrogenation generates CH
4The meaningless hydrogen consumption that causes.The off-line hydrogenation technique can be avoided the influence of gelatin liquefaction part unplanned shutdown to the stable hydrogenation device.As adopt online hydrogenation technique, and if gelatin liquefaction partly goes wrong, cause hydrogenation unit to stop in emergency, when temperature of reactor drops to below 100 ℃, the water in the gas phase can be absorbed by catalyzer, causes the catalyzer mechanical property to descend, and has a strong impact on catalyst life.
Principal feature of the present invention is the operating method that the stable hydrogenation main reactor adopts reverse flow.Liquefied coal coil enters from main reactor top, and hydrogen enters from the main reactor bottom, and the two reverse contact in reactor is reacted.The advantage of reverse flow reactor is that gas-to-liquid contact is abundant, reactor batch temperature is evenly distributed, and can improves the hydrodenitrification reaction atmosphere.Gas-to-liquid contact is improved reaction efficiency fully, also is difficult for producing undesired flow phenomenons such as channel; Because thermal discharge is very big in the liquefied coal coil stable hydrogenation reaction process, oil bed temperature rise when the gas coflow is very big, causes the reduction of catalyzer utilising efficiency, and reverse flow is because gas-liquid conversed mobile contact, thereby have more uniform bed temperature to distribute, catalyst utilization is improved.In addition, because the NH that the hydrodenitrification reaction generates
3But competitive adsorption produces restraining effect at catalyst hydrogenation denitrification activity center to further hydrodenitrification reaction, adopts the mode of reverse flow, and hydrogen constantly will react the NH that generates in the process of flowing that makes progress
3Upwards carry, weakened NH
3Competitive adsorption in catalyst active center has reduced NH to greatest extent
3To the restraining effect of hydrodenitrification, the reaction atmosphere of hydrodenitrification is improved, improved the utilising efficiency of catalyzer, can be implemented in than hydrodenitrification purpose under the mitigation condition.
Another distinguishing feature of the present invention is to increase guard reactor or stable hydrogenation main reactor top bed installs protective material additional as the protection bed before the stable hydrogenation main reactor, and the purpose that increases guard reactor or protection bed is that Primary Catalysts in the long-term operation process is active to keep stable in order to make.This is because liquefied coal coil contains a certain amount of metal and can't filter the less solid particulate matter of clean particle diameter, they easily are deposited on the Primary Catalysts top, cause reactor pressure reduction to occur, reduce hydrogenation unit running period, the metal that is deposited on simultaneously on the catalyzer can cause the hydrogenation catalyst permanent deactivation.
Below in conjunction with accompanying drawing method provided by the present invention is further detailed, but does not therefore limit present method.
Accompanying drawing is a liquefied coal coil adverse current stable hydrogenation process synoptic diagram provided by the invention.For using the situation of guard reactor, can not establish guard reactor in actual applications shown in the figure, and increase the protection bed on stable hydrogenation reactor bed top.
Method flow provided by the invention is as follows: the liquefied coal coil that comes out from the gelatin liquefaction unit takes the measure of starvation to be transported to the stock oil surge tank, install after filtration in the filtering and removing liquefied coal coil behind the entrained solid particle, after pipeline 1 incoming stock pump 2 boosts, through pipeline 3 and (effect of circulating hydrogen herein mainly is to prevent the pipeline coking) after part circulating hydrogen from pipeline 48 mixes, enter interchanger 5 through pipeline 4 and carry out heat exchange with vapor-phase reactant stream from pipeline 36, again through pipeline 6 with after circulating hydrogen from pipeline 51 mixes, entering guard reactor 8 through pipeline 7 contacts with the hydrogenation protecting agent, the logistics of coming out from guard reactor 8 enters stable hydrogenation reactor 10 through pipeline 9 top contacts with Hydrobon catalyst, circulating hydrogen then enters through the bottom of pipeline 11 from stable hydrogenation reactor 10, liquefied coal coil and hydrogen carry out hydrogenation reaction in stable hydrogenation reactor 10, the liquid phase reaction logistics of stable hydrogenation reactor 10 bottoms is the treated oil after the hydrotreatment, and the gas-phase reaction logistics then flows out from stable hydrogenation reactor 10 tops through pipeline 36; This gas-phase reaction logistics contains NH
3, H
2O, H
2S, lighter hydrocarbons and hydrogen, enter interchanger 5 through pipeline 36 and carry out heat exchange with liquefied coal coil raw material from pipeline 4, again through pipeline 37 with after water from pipeline 38 mixes, enter water washing tank 40 through pipeline 39, waste water is through pipeline 41 dischargers, hydrogen-rich gas then through pipeline 42 with after hydrogen-rich gas from pipeline 19 mixes, after pipeline 43 enters compressor 44 and boosts, be divided into two portions through pipeline 45, wherein a part through pipeline 46 with mix from the fresh hydrogen of pipeline 55 after, enter this reactor through pipeline 11 from the bottom of stable hydrogenation reactor 10 again; Another part then is divided into two-way again through pipeline 47; wherein one the tunnel through pipeline 48 with after liquefied coal coil from pipeline 3 mixes; enter interchanger 5 through pipeline 4, then mix after pipeline 7 enters guard reactor 8 with liquefied coal coil from pipeline 6 through pipeline 49, process furnace 50, pipeline 51 successively on another road.Fresh hydrogen enters interchanger 13 through pipeline 52, compressor 53, pipeline 54 successively and carries out heat exchange with treated oil from pipeline 12, again through pipeline 55 with after hydrogen-rich gas from pipeline 46 mixes, enter this reactor through pipeline 11 from the bottom of stable hydrogenation reactor 10.
Enter interchanger 13 and carry out heat exchange through pipeline 12 from stable hydrogenation reactor 10 effusive treated oils from the fresh hydrogen of pipeline 54, again through pipeline 14 with after water from pipeline 15 mixes, enter high-pressure separator 17 through pipeline 16, the hydrogen-rich gas at high-pressure separator 17 tops with after hydrogen-rich gas from pipeline 42 mixes, enters compressor 44 through pipeline 43 through pipeline 19; The waste water of high-pressure separator 17 bottoms is through pipeline 18 dischargers; The logistics of high-pressure separator 17 bottoms then enters light pressure separator 21 through pipeline 20, the gas at light pressure separator 21 tops is through pipeline 22 emptying, the waste water of light pressure separator 21 bottoms is through pipeline 23 dischargers, and the logistics of light pressure separator 21 bottoms then enters separation column 25 through pipeline 24.The logistics at separation column 25 tops enters separator 29 through pipeline 26, condenser 27, pipeline 28 successively, LPG is through pipeline 30 caterpillars, naphtha fraction through pipeline 31 with from the naphtha fraction on separation column 25 tops through pipeline 32 caterpillars, the tail oil cut of separation column 25 bottoms is through pipeline 34 caterpillars, wherein part tail oil cut can through pipeline 35 with from the diesel oil distillate of separation column 25 bottoms through pipeline 33 caterpillars.
The present invention adopts the stable hydrogenation of off-line to liquefied coal coil, the stable hydrogenation reactor adopts the operating method of reverse flow, gas-to-liquid contact is abundant, reactor temperature is evenly distributed, improved reaction atmosphere, the utilising efficiency of catalyzer is improved, and can be implemented in the hydrodenitrification of liquefied coal coil under the relative mitigation reaction conditions.
The following examples will give further instruction to present method, but therefore not limit present method.
Used liquefied coal coil A, B, C are all through filtering among the embodiment; the Hydrobon catalyst trade names are RN-2; hydrogenation protecting agent trade names are RG-10A/RG-10B, produce by Sinopec Chang Ling catalyst plant, and the volume ratio of RG-10A/RG-10B and RN-2 is 0.2.Test is carried out on medium-sized fixed bed hydrogenation device.
Embodiment 1
Test raw material is liquefied coal coil A, and stock oil character, processing condition and product property are listed in table 1, table 2 and table 3 respectively.As seen from Table 3, the bromine valency of stable hydrogenation product is very low, shows that the alkene major part is by saturated in the liquefied coal coil; The content of product nitrogen and sulphur is low, and boiling range lightens, and has reached the purpose of stable hydrogenation.
Embodiment 2
Test raw material is liquefied coal coil B, and stock oil character, processing condition and product property are listed in table 1, table 2 and table 3 respectively.By table as seen, raw material nitrogen content height, under the operational condition of harshness, stable hydrogenation product bromine valency is very low, shows that alkene major part in the liquefied coal coil is by saturated; The content of product nitrogen and sulphur is low, and boiling range lightens, and has reached the purpose of stable hydrogenation.
Embodiment 3
Test raw material is liquefied coal coil C, and stock oil character, processing condition and product property are listed in table 1, table 2 and table 3 respectively.By table as seen, stable hydrogenation product bromine valency is very low, shows that alkene major part in the liquefied coal coil is by saturated; The content of product nitrogen and sulphur is low, and boiling range lightens, and has reached the purpose of stable hydrogenation.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| The liquefied coal coil numbering | ??????A | ??????B | ??????C |
| Density (20 ℃), g/cm 3 | ????0.9870 | ????0.9429 | ????0.9380 |
| S，m％ | ????0.15 | ????0.60 | ????0.42 |
| N，m％ | ????0.65 | ????1.1 | ????0.85 |
| Oxygen level, m% | ????25.0 | ????21.4 | ????18.8 |
| The bromine valency, gBr/100g | ????2.4 | ????2.1 | ????1.58 |
| Boiling range ASTM D-1160, ℃ | |||
| Initial boiling point | ????109 | ????152 | ????147 |
| ??10％ | ????141 | ????217 | ????180 |
| ??50％ | ????321 | ????318 | ????336 |
| ??95％ | ????453 | ????411 | ????427 |
| Do | ????475 | ????460 | ????445 |
Table 2
| Processing condition | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Temperature of reaction, ℃ | ????345 | ????348 | ????346 |
| The hydrogen dividing potential drop, MPa | ????14.0 | ????15.0 | ????12.0 |
| Volume space velocity, h -1 | ????1.5 | ????1.5 | ????1.0 |
| Hydrogen-oil ratio, v/v | ????1000 | ????1400 | ????1300 |
Table 3
| Product characteristics | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Density (20 ℃), g/cm 3 | ????0.9020 | ????0.8872 | ????0.8889 |
| S，ppm | ????58 | ????187 | ????182 |
| N，ppm | ????127 | ????162 | ????204 |
| The bromine valency, gBr/100g | ????0.57 | ????0.69 | ????0.88 |
| Oxygen level, m% | ????＜0.3 | ????＜0.3 | ????＜0.3 |
| Boiling range ASTM D-86, ℃ | |||
| Initial boiling point | ????97 | ????80 | ????123 |
| ??10％ | ????125 | ????174 | ????169 |
| ??50％ | ????298 | ????308 | ????311 |
| ??95％ | ????434 | ????401 | ????416 |
| Do | ????468 | ????453 | ????441 |
Claims (6)
1, a kind of liquefied coal coil adverse current stable hydrogenation process, liquefied coal coil after it is characterized in that filtering and hydrogen enter the stable hydrogenation reactor from the upper and lower of reactor respectively, contact with hydrogenation protecting agent, Hydrobon catalyst, the stable hydrogenation reactor effluent passes through high-pressure separator, light pressure separator, separation column successively, separates to obtain lighting end and tail oil cut; Mix with fresh hydrogen from the isolated hydrogen rich stream of high-pressure separator, loop back the stable hydrogenation reactor.
2,, it is characterized in that described liquefied coal coil boiling range is C according to the method for claim 1
5～500 ℃.
3,, it is characterized in that reaction conditions is: hydrogen dividing potential drop 3.0～30.0MPa according to the method for claim 1; 270～450 ℃ of temperature of reaction; Liquid hourly space velocity 0.1～10h
-1, hydrogen-oil ratio 300～2800v/v.
4,, it is characterized in that described hydrogenation protecting agent is VIB or the VIII family non-precious metal catalyst that loads on unformed aluminum oxide or the silica-alumina supports according to the method for claim 1.
5,, it is characterized in that described described Hydrobon catalyst is VIB or the VIII family non-precious metal catalyst that loads on unformed aluminum oxide or the silica-alumina supports according to the method for claim 1.
6, according to the method for claim 1, the volume ratio that it is characterized in that described hydrogenation protecting agent and hydrofining agent is 0.03～0.35.
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| CN 03126443 CN1600837A (en) | 2003-09-28 | 2003-09-28 | Steady hydrogenation method in counter current of oil liquefied from coal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378201C (en) * | 2005-07-15 | 2008-04-02 | 中国石油化工股份有限公司 | Stabilized hydrogenation of coal liquefied oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100378201C (en) * | 2005-07-15 | 2008-04-02 | 中国石油化工股份有限公司 | Stabilized hydrogenation of coal liquefied oil |
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