CN101962571A - Coal tar heavy fraction suspension-bed hydrocracking method and system thereof - Google Patents
Coal tar heavy fraction suspension-bed hydrocracking method and system thereof Download PDFInfo
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- CN101962571A CN101962571A CN201010525146XA CN201010525146A CN101962571A CN 101962571 A CN101962571 A CN 101962571A CN 201010525146X A CN201010525146X A CN 201010525146XA CN 201010525146 A CN201010525146 A CN 201010525146A CN 101962571 A CN101962571 A CN 101962571A
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- 239000011280 coal tar Substances 0.000 title claims abstract description 65
- 238000004517 catalytic hydrocracking Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000001257 hydrogen Substances 0.000 claims abstract description 50
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 50
- 239000003921 oil Substances 0.000 claims abstract description 47
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 9
- 239000003502 gasoline Substances 0.000 claims abstract description 7
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 6
- 239000000295 fuel oil Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 15
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- 238000005987 sulfurization reaction Methods 0.000 claims description 14
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- 239000011269 tar Substances 0.000 claims description 10
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- 239000012071 phase Substances 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 239000007792 gaseous phase Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 4
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005194 fractionation Methods 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
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- 238000010008 shearing Methods 0.000 claims description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 6
- 239000003245 coal Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- -1 aromatic hydroxy compound Chemical class 0.000 description 1
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Abstract
The invention belongs to the technical field of coal chemical industry, and provides a coal tar heavy fraction suspension-bed hydrocracking method. The method comprises the following steps: mixing raw materials of coal tar heavy fractions with a catalyst and a vulcanizing agent to form a uniform mixed material; vulcanizing the catalyst in the mixed material under the action of hydrogen; preheating the vulcanized mixed material, and then allowing the preheated material to enter a suspension-bed reactor for hydrocracking reaction; and fractionating the product from the suspension-bed reactor to finally obtain gaseous hydrocarbon, gasoline fractions, diesel fractions and tail oil. In the invention, by directly adopting the hydrocracking method with a coal tar heavy fraction suspension bed and a system thereof, the coal tar heavy fractions can keep light weight, and the yield of the fuel oil product hydrogenated by coal tar can be effectively increased; and the suspension-bed hydrogenation reactor has simple structure without a bed layer, thus causing no phenomena such as blockage, increased pressure drop, overtemperature and the like occurred on the reaction bed layer, and the reactor further has the characteristics of great operation flexibility, long operation cycle, being safe and stable, easy control and the like.
Description
Technical field
The invention belongs to technical field of coal chemical industry, be specifically related to the method and system of coal tar heavy fractioning floating bed hydrocracking.
Background technology
In the coal tar course of processing, generally with in the coal tar 〉=cut is called last running more than 350 ℃.Coal tar heavy fractioning mainly is made up of aromatic hydrocarbon, colloid, bituminous matter and impurity etc., mostly is the above aromatic hydroxy compound of three rings and Fourth Ring, and density is greater than 1.0g/cm
3, wherein nitrogen content, oxygen level and foreign matter content are all higher.As far back as 1938, Germany was raw material with tar from lignite last running (〉=325 ℃ of cuts) just, has carried out the suitability for industrialized production of floating bed hydrocracking, adopted Fe(OH)
2-semicoke is a catalyzer, and working pressure is that 30MPa, temperature of reaction are 465～470 ℃.Nineteen fifty-nine, China Fushun No.3 Petroleum Factory was a raw material with bituminous coal semi coking tar last running (〉=325 ℃ of cuts), at 20MPa, 460～480 ℃, MoO
3Under-semicoke the catalyst action, carried out the suitability for industrialized production of floating bed hydrocracking.The subject matter of above-mentioned technology is that reaction pressure and temperature are too high, and the catalyst system therefor activity is low, consumption is big, and granules of catalyst is excessive in addition, is difficult to aborning separate, and easily causes equipment and line clogging.In patent ZL02122573.7 (2008-08-20), be that the full cut of coal tar is removed less than C through flash distillation earlier
5Behind the hydrocarbon, carry out pre-hydrofining by 4 switch protecting reactors again, enter the floating bed hydrogenation reactor then, at MoO
3-WO
3-NiO-P-TiO
2Under the catalyst action, the hydrogenator inlet pressure is not more than 15.0MPa(hydrogen dividing potential drop), initial reaction temperature is 300～390 ℃ (beds medial temperature), volume space velocity 0.4～4.0h
-1, hydrogen-oil ratio 500～3000Nm
3/ m
3This production method is actual to be fixed bed and suspension bed process integration process, but owing to foreign matter content height in the tar, the bed choking phenomenon takes place easily, keep long-term operation, often need more catalyst changeout, catalyst levels is big, increase cost, made complex process, increased equipment and process cost.Switch the moisture that product that reactor comes out contains a great deal of in addition, the unprocessed hydrogenator that directly enters, very big to catalyzer (catalyzer that especially contains molecular sieve) activity influence, can cause catalyst activity to reduce greatly.(Jemes H E such as Australian H E Jemes in 1987, Schluter k, Relph J T.Upgrading of flash pyrolysis tars to synthetic crude oil.4.Hydrotreatment with iron catalyst in a slurry-phase reactor.Fuel, 1987,66:637-642.) be raw material with the full cut of bituminous coal semi coking tar, carried out the research of floating bed hydrocracking.With red mud and the red mud after handling make catalyzer, reaction pressure is that 13.8MPa, temperature of reaction are that 419～462 ℃, hydrogen-oil ratio are 3.2Nm
3/ kg, tar air speed are 0.45h
-1Result of study shows, product oil phase to density up to 0.98, C
1～C
4The hydrocarbon gas productive rate is 10%～13.4%, and it is lower to generate oily productive rate.Patent CN1766058A (2006-05-03) directly carries out floating bed hydrogenation to the full cut of coal tar and introduces.Adopting homogeneous catalyst is the compound or the aqueous solution of periodic table of elements VI B, VII B and one or more metals of VIII family, wherein preferably for containing the material of metallic elements such as Mo, Ni, Co, W, Cr, Fe.The total add-on of catalyzer is counted 50～200 μ g/g with metal.Floating bed hydrogenation is handled and the condition of lighting is: 320～420 ℃ of temperature, pressure 6～18MPa, liquid hourly space velocity 0.5～3.0 h
-1, hydrogen to oil volume ratio 400～2000.Owing to contain in the full cut of above-mentioned coal tar less than 350 ℃ of lighting ends in the past, in the floating bed hydrocracking reaction, easily generate the hydrocarbon gas product, its productive rate is also higher, thereby having reduced the productive rate of purpose product petroleum naphtha or gasoline fraction, diesel oil distillate, is unreasonable from Technological Economy.Patent CN101240191A(2008-08-13) and patent CN101240192A(2008-08-13) provide a kind of coal tar heavy fractioning to produce the method for light-weight fuel oil and fine-quality diesel oil, these two patents adopt hydrofining-hydrocracking combined process and hydrofining-hydrocracking-upgrading combination process, all adopt fixed bed hydrogenation.Because the coking at high temperature of coal tar heavy duty component is very fast, bed is stopped up, cause bed layer pressure to increase, make production operation be difficult to control, overheating problem also easily takes place in addition, greatly reduce the work-ing life of catalyzer.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of coal tar heavy fractioning suspension bed hydrocracking method, coal tar heavy fractioning is directly carried out floating bed hydrocracking, have that technical process is simple, transformation efficiency is high, characteristics of running safety and stability, easy to operate and control.The present invention also provides coal tar heavy fractioning floating bed hydrocracking system in addition, and equipment layout is reasonable, compact, easy handling.
The technical scheme that the present invention is adopted for achieving the above object is: the coal tar heavy fractioning suspension bed hydrocracking method is mixed into even mixed materials with raw material coal tar heavy fractioning and catalyzer and vulcanizing agent; Under the effect of hydrogen, the catalyzer in the mixture is vulcanized; Mixture after the sulfuration carries out preheating, enters suspended-bed reactor then and carries out hydrocracking reaction; The product that is come out by suspended-bed reactor obtains hydrocarbon gas (C through fractionation
1～C
4), gasoline fraction (C
5～160 ℃ of cuts), diesel oil distillate (160～350 ℃), tail oil (greater than 350 ℃).
The tail oil that described fractionation obtains, a part turns back to recycle in the preliminary heating device as the circulation tail oil, and another part tail oil is sent as the output tail oil.
Described coal tar heavy fractioning is: coalite tar last running, coal-tar middle oil last running, middle coalite tar last running, coal-tar heavy oil last running.
Described catalyzer adopts water-soluble homogeneous catalyst, adds rare earth element ce; The composition of catalyzer: Mo content is 4%～12%, is preferably 6%～8%; Ni content is 0.1%～1%, is preferably 0.3%～0.7%; Ce content is 0.1%～0.8%, is preferably 0.3%～0.6%; P content is 0.2%～0.8%, is preferably 0.3%～0.5%.Catalyzer is 100～800 μ gg in the total add-on of metal
-1, be preferably 200～500 μ gg
-1(quality with the raw material coal tar heavy fractioning is a base of calculation).
Described vulcanizing agent is the material of various sulfur-bearings, as sulphur, dithiocarbonic anhydride (CS
2), dimethyl thioether (DMS), a kind of in the dimethyl disulphide (DMDS) etc., the add-on of vulcanizing agent is 0.05%～0.8%, being preferably 0.1%～0.5%(is base of calculation with the quality of raw material coal tar heavy fractioning).
Step up cure is adopted in described sulfuration: pressure is 0.3～0.7MPa during first stage cure, preferred 0.4～0.6MPa, and 200～240 ℃ of temperature, the air speed of raw material coal tar heavy fractioning in vulcanizing apparatus is 0.2～0.5 h
-1(effective volume with vulcanizing apparatus serves as to calculate benchmark); Identical with first stage cure pressure and air speed during the subordinate phase sulfuration, curing temperature is 300～360 ℃.The sulfuration feeding manner adopts the charging of mixture downflow system mode, and hydrogen upflowing mode enters, and the two forms counter current contact; Also can adopt and flow to the material form; Hydrogen to oil volume ratio is 350～950.
Preheating temperature is 360～430 ℃ during described preheating, the reaction of floating bed hydrocracking: pressure 8～16MPa, 380～450 ℃ of temperature, liquid hourly space velocity 0.5～2.5 h
-1, hydrogen to oil volume ratio is 900～1600.
Coal tar heavy fractioning floating bed hydrocracking of the present invention system, (mixing tank can be multistage shearing pump to mixing tank, strong mixer, emulsor and colloidal mill etc.) outlet connection vulcanizing apparatus opening for feed, vulcanizing apparatus also has the pressure hydrogen inlet, the vulcanizing apparatus discharge port is communicated with the preheating oven opening for feed, the preheating oven discharge port is communicated with the suspended-bed reactor opening for feed, the suspended-bed reactor discharge port is communicated with the high-pressure separator opening for feed, the high-pressure separator gaseous phase outlet is communicated with the High Pressure Hydrogen supply arrangement, the High Pressure Hydrogen supply arrangement is communicated with the preheating oven opening for feed, the outlet of high-pressure separator liquid phase is communicated with separation column, and separation column connects each run tank.
A described separation column tail oil outlet part connects the tail oil collector, and a part is through being equipped with the pipeline connection preheating oven opening for feed of tail oil recycle pump.
Described high-pressure separator gaseous phase outlet is through being equipped with the pipeline connection High Pressure Hydrogen supply arrangement of circulating hydrogen compressor.
Described vulcanizing apparatus pneumatic outlet is through being equipped with the pipeline connection pressure hydrogen supply arrangement of condensation separator, and the pressure hydrogen supply arrangement is communicated with vulcanizing apparatus pressure hydrogen inlet.
The present invention adopts the coal tar heavy fractioning suspension bed directly to carry out the method and system of hydrocracking, can make the coal tar heavy fractioning lighting, effectively improves the productive rate that coal tar hydrogenating generates fuel oil.The floating bed hydrogenation structure of reactor is simple, does not have bed, does not have phenomenons such as reactor bed obstruction, pressure drop increase and overtemperature.And have that turndown ratio is big, on-stream time length, safety and stability, characteristics such as easy to control.
The coal tar suspension bed hydrocracking system design of the present invention is reasonable, the equipment layout compactness, adopt reverse-flow charging as vulcanizing equipment, mixture from the top of vulcanization reaction device with the charging of downflow system mode, hydrogen enters in the upflowing mode from vulcanization reaction device bottom, the two forms counter current contact, helps the tight cure of catalyzer.Can certainly adopt the cocurrent cooling operation form.Product in the system in time carries out recycle and reuse, saves cost.
Description of drawings:
Fig. 1 directly carries out the process flow sheet of suspension bed hydrocracking method and system for coal tar heavy fractioning of the present invention.
Among the figure: the 1st, coal tar heavy fractioning, the 2nd, catalyzer, the 3rd, vulcanizing agent, the 4th, mixing tank, the 5th, high-pressure pump, the 6th, pressure hydrogen, the 7th, vulcanizing apparatus, the 8th, condensation separator, the 9th, water, the 10th, rich hydrogen circulates, the 11st, charging high-pressure pump, the 12nd, preheating oven, the 13rd, High Pressure Hydrogen, the 14th, suspended-bed reactor, the 15th, high-pressure separator, the 16th, recycle hydrogen, the 17th, circulating hydrogen compressor, the 18th, separation column, the 19th, C
1～C
4Hydrocarbon gas, the 20th, C
5～160 ℃ gasoline fraction, 21 is diesel oil distillates of 160～350 ℃, the 22nd, greater than 350 ℃ tail oil, the 23rd, circulation tail oil, the 24th, tail oil recycle pump, the 25th, output tail oil.
Embodiment:
Coal tar heavy fractioning floating bed hydrocracking system as shown in Figure 1: adopt multistage shearing pump, strong mixer, mixing tank such as emulsor and colloidal mill batch mixing, the opening for feed of the pipeline connection vulcanizing apparatus 7 of mixture discharge port through high-pressure pump 5 is installed, after the pipeline of the pneumatic outlet of vulcanizing apparatus through condensation separator 8 is installed told water 9, Fu Qing returns the pressure hydrogen supply arrangement, the pressure hydrogen supply arrangement is communicated with the pressure hydrogen inlet of vulcanizing apparatus 7, the pipeline of vulcanizing apparatus 7 discharge ports through high-pressure pump 11 is installed is communicated with the preheating oven opening for feed, high pressure hydrogen 13, recycle hydrogen 16, circulation tail oil 23 also is communicated with the preheating oven opening for feed respectively, preheating oven 12 discharge ports are communicated with suspended-bed reactor 14 opening for feeds, the suspended-bed reactor discharge port is communicated with high-pressure separator 15 opening for feeds, the gaseous phase outlet of high-pressure separator 15 is through being equipped with the pipeline connection High Pressure Hydrogen supply arrangement recycle of circulating hydrogen compressor 17, the liquid phase outlet of high-pressure separator 15 is communicated with the separation column opening for feed, and the separation column fraction products is C
1～C
4Hydrocarbon gas 19, C
520,160～350 ℃ of diesel oil distillates 21 of～160 ℃ of gasoline fractions, greater than 350 ℃ tail oils 22, the part in the tail oil 22 is returned preheating oven 12 opening for feeds as circulation tail oil 23 by the pipeline that tail oil recycle pump 24 is housed, and another part is sent for output tail oil 25.
In order to further specify coal tar heavy fractioning suspension bed hydrocracking method of the present invention and system, be illustrated with the following Examples, but the invention is not restricted to these embodiment.
Below the per-cent that relates among each embodiment be mass percent (m%).The character of the coal tar heavy fractioning (〉=350 ℃ of cuts) that experiment is used is as shown in table 1.
Table 1 coal tar heavy fractioning (〉=350 ℃ of cuts) character
Embodiment 1～4:
Adopt above-mentioned coal tar heavy fractioning floating bed hydrocracking system shown in Figure 1, coal tar heavy fractioning 1, catalyzer 2 and vulcanizing agent 3 are sent into mixing tank 4 in required ratio, in mixing tank, carry out uniform mixing with strong mixer, mixture sent in the vulcanizing apparatus 7 by high-pressure pump 5 vulcanize the recycle after condensation separator 8 is told water 9 of the rich hydrogen 10 in the sulfidation.Circulate rich hydrogen 10 with enter vulcanizing apparatus 7 after pressure hydrogen 6 is mixed, the material that vulcanizing apparatus 7 comes out through high-pressure pump 11 with enter preheating oven 12 after high pressure hydrogen 13, recycle hydrogen 16, circulation tail oil 23 mix, material after the preheating is sent into and is carried out hydrocracking reaction in the suspended-bed reactor 14, resultant of reaction is sent into and is carried out the solution-air separation in the high-pressure separator 15, separated hydrogen 16 is through circulating hydrogen compressor 17 recycles, separated products oil is sent into separation column 18 and is separated, and its product is C
1～C
4Hydrocarbon gas 19, C
520,160～350 ℃ of diesel oil distillates 21 of～160 ℃ of gasoline fractions, greater than 350 ℃ tail oils 22, the part in the tail oil 22 is returned preheating oven 12 as circulation tail oil 23 by tail oil recycle pump 24, and another part is output tail oil 25.4 kinds of coal tar heavy fractioning add-ons are 10kg/h in the test, and catalyzer consists of Mo7%, Ni0.5%, Ce0.4%, P0.3%; 4 kinds of mixtures are all at 0.5MPa, 230 ℃, air speed 0.3h
-1Under the condition catalyzer is carried out first stage cure, be warmed up to 310 ℃ then, carry out the subordinate phase sulfuration under above-mentioned the same terms, hydrogen to oil volume ratio is 800 in sulfidation.Adopt CS
2Be vulcanizing agent, add-on is that 0.5%(serves as to calculate benchmark with the coal tar heavy fractioning quality).The preheating temperature of sulfuration back material is 360 ℃, floating bed hydrocracking test reaction conditions and the results are shown in Table shown in 2.
Table 2 floating bed hydrocracking test reaction conditions and result
Embodiment 5～8:
Adopt above-mentioned coal tar heavy fractioning floating bed hydrocracking system shown in Figure 1, test method is identical with the foregoing description 1～4 with process.
4 kinds of coal tar heavy fractioning add-ons are 15kg/h in the test, and catalyzer consists of Mo8%, Ni0.4%, Ce0.3%, P0.4%; 4 kinds of mixtures are all at 0.6MPa, 240 ℃, air speed 0.4h
-1Carry out first stage cure under the condition, be warmed up to 330 ℃ then, under above-mentioned the same terms, carry out the subordinate phase sulfuration.Hydrogen to oil volume ratio is 600 in sulfidation, and employing DMS is a vulcanizing agent, and add-on is that 0.3%(serves as to calculate benchmark with the coal tar heavy fractioning quality).The preheating temperature of sulfuration back material is 370 ℃, floating bed hydrocracking test reaction conditions and the results are shown in Table shown in 3.
Table 3 floating bed hydrocracking test reaction conditions and result
Embodiment 9～12:
Adopt above-mentioned coal tar heavy fractioning floating bed hydrocracking system shown in Figure 1, test method is identical with the foregoing description 1～4 with process.
The coal tar heavy fractioning add-on is 20kg/h in the test, and catalyzer consists of Mo6%, Ni0.6%, Ce0.5%, P0.5%; 4 kinds of mixtures are all at 0.4MPa, 200 ℃, air speed 0.2h
-1Carry out first stage cure under the condition, be warmed up to 340 ℃ then, under above-mentioned the same terms, carry out the subordinate phase sulfuration.Hydrogen to oil volume ratio is 700 in sulfidation, and employing DMDS is a vulcanizing agent, and add-on is that 0.4%(serves as to calculate benchmark with the coal tar heavy fractioning quality).The preheating temperature of sulfuration back material is 380 ℃, floating bed hydrocracking test reaction conditions and the results are shown in Table shown in 4.
Table 4 floating bed hydrocracking test reaction conditions and result
Claims (10)
1. coal tar heavy fractioning suspension bed hydrocracking method is characterized in that: raw material coal tar heavy fractioning and catalyzer and vulcanizing agent are mixed into even mixed materials; Under the effect of hydrogen, the catalyzer in the mixture is vulcanized; Mixture after the sulfuration carries out preheating, enters suspended-bed reactor then and carries out hydrocracking reaction; The product that is come out by suspended-bed reactor obtains hydrocarbon gas, gasoline fraction, diesel oil distillate, tail oil through fractionation.
2. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1 is characterized in that: the tail oil that fractionation obtains, and a part turns back to recycle in the preheating oven as the circulation tail oil, and another part tail oil is sent as the output tail oil.
3. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1 is characterized in that: coal tar heavy fractioning is: coalite tar last running, coal-tar middle oil last running, middle coalite tar last running, coal-tar heavy oil last running.
4. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1 is characterized in that: catalyzer adopts water-soluble homogeneous catalyst, adds rare earth element ce; The composition of catalyzer: Mo content is 4%～12%, is preferably 6%～8%; Ni content is 0.1%～1%, is preferably 0.3%～0.7%; Ce content is 0.1%～0.8%, is preferably 0.3%～0.6%; P content is 0.2%～0.8%, is preferably 0.3%～0.5%;
Catalyzer is 100～800 μ gg in the total add-on of metal
-1, be preferably 200～500 μ gg
-1(quality with the raw material coal tar heavy fractioning is a base of calculation).
5. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1, it is characterized in that: vulcanizing agent is the material of various sulfur-bearings, as sulphur, dithiocarbonic anhydride, dimethyl thioether, a kind of in the dimethyl disulphide etc., the add-on of vulcanizing agent is 0.05%～0.8%, and being preferably 0.1%～0.5%(is base of calculation with the quality of raw material coal tar heavy fractioning).
6. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1, it is characterized in that: step up cure is adopted in sulfuration: pressure is 0.3～0.7MPa during first stage cure, preferred 0.4～0.6MPa, 200～240 ℃ of temperature, the air speed of raw material coal tar heavy fractioning in vulcanizing apparatus is 0.2～0.5 h
-1(effective volume with vulcanizing apparatus serves as to calculate benchmark); Identical with first stage cure pressure and air speed during the subordinate phase sulfuration, curing temperature is 300～360 ℃;
The sulfuration feeding manner adopts the charging of mixture downflow system mode, and hydrogen upflowing mode enters, and the two forms counter current contact; Also can adopt and flow to the material form; Hydrogen to oil volume ratio is 350～950.
7. coal tar heavy fractioning suspension bed hydrocracking method according to claim 1 is characterized in that: preheating temperature is 360～430 ℃ during preheating, the reaction of floating bed hydrocracking: pressure 8～16MPa, 380～450 ℃ of temperature, liquid hourly space velocity 0.5～2.5 h
-1, hydrogen to oil volume ratio is 900～1600.
8. coal tar heavy fractioning floating bed hydrocracking system, it is characterized in that: (mixing tank can be multistage shearing pump to mixing tank, strong mixer, emulsor and colloidal mill etc.) outlet connection vulcanizing apparatus opening for feed, vulcanizing apparatus also is provided with the pressure hydrogen inlet, the vulcanizing apparatus discharge port is communicated with the preheating oven opening for feed, the preheating oven discharge port is communicated with the suspended-bed reactor opening for feed, the suspended-bed reactor discharge port is communicated with the high-pressure separator opening for feed, the high-pressure separator gaseous phase outlet is communicated with the High Pressure Hydrogen supply arrangement, the High Pressure Hydrogen supply arrangement is communicated with the preheating oven opening for feed, the outlet of high-pressure separator liquid phase is communicated with separation column, and separation column connects each run tank.
9. coal tar heavy fractioning floating bed hydrocracking according to claim 8 system is characterized in that: a separation column tail oil outlet part connects the tail oil collector, and a part is through being equipped with the pipeline connection preheating oven opening for feed of tail oil recycle pump.
10. coal tar heavy fractioning floating bed hydrocracking according to claim 8 system, it is characterized in that: the high-pressure separator gaseous phase outlet is through being equipped with the pipeline connection High Pressure Hydrogen supply arrangement of circulating hydrogen compressor; The vulcanizing apparatus pneumatic outlet is through being equipped with the pipeline connection pressure hydrogen supply arrangement of condensation separator, and the pressure hydrogen supply arrangement is communicated with vulcanizing apparatus pressure hydrogen inlet.
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| CN102719271A (en) * | 2012-07-12 | 2012-10-10 | 韩钊武 | Method for preparing diesel by high-temperature coal tar through hydrogenation |
| CN103265971A (en) * | 2013-05-15 | 2013-08-28 | 煤炭科学研究总院 | Heterogeneous coal tar suspension bed hydrogenation method |
| CN103540351A (en) * | 2012-07-12 | 2014-01-29 | 中国石油天然气股份有限公司 | Combined process method for treating coal tar whole fraction |
| CN103789026A (en) * | 2014-01-29 | 2014-05-14 | 河南龙成煤高效技术应用有限公司 | Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst |
| CN105623703A (en) * | 2016-01-19 | 2016-06-01 | 何巨堂 | Thermal high-pressure dissociating gas dust removal method for three-phase product of hydrocarbon material hydrogenation reaction |
| CN105754648A (en) * | 2016-04-22 | 2016-07-13 | 北京神雾环境能源科技集团股份有限公司 | Coal tar processing method and system |
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| CN108264933A (en) * | 2016-12-30 | 2018-07-10 | 北京华石联合能源科技发展有限公司 | A kind of device that heavy oil lighting is realized using floating bed hydrogenation technology |
| CN109082299A (en) * | 2018-09-25 | 2018-12-25 | 孙志良 | A kind of coal tar hydrocracking decomposition technique |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
| WO2020186638A1 (en) * | 2019-03-15 | 2020-09-24 | 南京延长反应技术研究院有限公司 | Heavy oil hydrogenation and micro-interface strengthened suspension bed reaction system and method |
| US10889770B2 (en) | 2016-12-30 | 2021-01-12 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method and device for lightening heavy oil by utilizing a suspension-bed hydrogenation process |
| CN112391200A (en) * | 2020-10-22 | 2021-02-23 | 中国科学院大连化学物理研究所 | Method for hydrogenating ethylene cracking tar |
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| CN102719271A (en) * | 2012-07-12 | 2012-10-10 | 韩钊武 | Method for preparing diesel by high-temperature coal tar through hydrogenation |
| CN103540351A (en) * | 2012-07-12 | 2014-01-29 | 中国石油天然气股份有限公司 | Combined process method for treating coal tar whole fraction |
| CN103265971A (en) * | 2013-05-15 | 2013-08-28 | 煤炭科学研究总院 | Heterogeneous coal tar suspension bed hydrogenation method |
| WO2014183429A1 (en) * | 2013-05-15 | 2014-11-20 | 煤炭科学研究总院 | Heterogeneous suspension-bed hydrogenation method for coal-based oil product |
| CN103265971B (en) * | 2013-05-15 | 2015-03-25 | 煤炭科学研究总院 | Heterogeneous coal tar suspension bed hydrogenation method |
| CN103789026A (en) * | 2014-01-29 | 2014-05-14 | 河南龙成煤高效技术应用有限公司 | Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst |
| CN105623703A (en) * | 2016-01-19 | 2016-06-01 | 何巨堂 | Thermal high-pressure dissociating gas dust removal method for three-phase product of hydrocarbon material hydrogenation reaction |
| CN105754648B (en) * | 2016-04-22 | 2018-02-27 | 神雾科技集团股份有限公司 | Coal tar processing method and its system |
| CN105754648A (en) * | 2016-04-22 | 2016-07-13 | 北京神雾环境能源科技集团股份有限公司 | Coal tar processing method and system |
| CN106281427A (en) * | 2016-10-14 | 2017-01-04 | 北京神雾环境能源科技集团股份有限公司 | A kind of system and method that coal tar is processed |
| CN106745397A (en) * | 2016-12-28 | 2017-05-31 | 西安建筑科技大学 | The efficient removal device of oil pollutant and method in a kind of coal chemical industrial waste water |
| CN106745397B (en) * | 2016-12-28 | 2023-03-21 | 西安建筑科技大学 | Efficient removing device and method for oil pollutants in coal chemical industry wastewater |
| CN108264933A (en) * | 2016-12-30 | 2018-07-10 | 北京华石联合能源科技发展有限公司 | A kind of device that heavy oil lighting is realized using floating bed hydrogenation technology |
| CN108264933B (en) * | 2016-12-30 | 2020-03-17 | 北京华石联合能源科技发展有限公司 | Device for realizing heavy oil lightening by using suspension bed hydrogenation technology |
| US10889770B2 (en) | 2016-12-30 | 2021-01-12 | Beijing Huashi United Energy Technology And Development Co., Ltd. | Method and device for lightening heavy oil by utilizing a suspension-bed hydrogenation process |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
| CN109913252B (en) * | 2017-12-13 | 2020-12-08 | 中国石油化工股份有限公司 | Coal tar combined hydrogenation process starting method |
| CN109082299A (en) * | 2018-09-25 | 2018-12-25 | 孙志良 | A kind of coal tar hydrocracking decomposition technique |
| WO2020186638A1 (en) * | 2019-03-15 | 2020-09-24 | 南京延长反应技术研究院有限公司 | Heavy oil hydrogenation and micro-interface strengthened suspension bed reaction system and method |
| CN112391200A (en) * | 2020-10-22 | 2021-02-23 | 中国科学院大连化学物理研究所 | Method for hydrogenating ethylene cracking tar |
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