CN104927917A - Method for producing high-boiling-point aromatic solvent oil through heavy benzol lightening - Google Patents
Method for producing high-boiling-point aromatic solvent oil through heavy benzol lightening Download PDFInfo
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- CN104927917A CN104927917A CN201510316101.4A CN201510316101A CN104927917A CN 104927917 A CN104927917 A CN 104927917A CN 201510316101 A CN201510316101 A CN 201510316101A CN 104927917 A CN104927917 A CN 104927917A
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Abstract
The invention belongs to the technical field of the coal chemical industry and relates to a production method of aromatic solvent oil, particularly to a method for producing high-boiling-point aromatic solvent oil through heavy benzol lightening. According to the invention, heavy benzol is adopted as a raw material, sequentially passes through a prehydrogenation reactor, a hydrocracking reactor and a hydrorefining reactor under action of a catalyst and is then subjected to rectification and separation, and fractions at 150-180 DEG C and at 180-215 DEG C are taken to obtain solvent oil products of corresponding distillation range sections. The invention aims to perform hydrocracking on arene with two or more rings so as to produce mono-aromatic hydrocarbon, so that the density of hydrogenated oil products is effectively reduced, the distillation range of the oil products is remarkably removed to the low-temperature direction, and the obvious lightening effect is realized. The heavy benzol raw material is directly subjected to hydrotreatment without the complicated raw material separation step, so that the cost and energy consumption are reduced, and the prepared high-boiling-point aromatic oil meets the national standard. According to the invention, a novel effective path is provided for promoting refined utilization of coal tar and relieving exhaustion of petroleum resources.
Description
Technical field
The invention belongs to technical field of coal chemical industry, relate to the production method of aromatic solvent naphtha, refer more particularly to a kind of method that high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting.
Background technology
As one of main petroleum products, solvent oil is together with gasoline, kerosene, diesel oil, lubricating oil and be called the large class petroleum products of China five.Solvent oil has a wide range of applications in industries such as medicine, chemical industry, macromolecular material, rubber and paint.At present, the main raw material that solvent oil is produced has three sources: crude oil straight run, and catalytic reforming is raffinated oil and condensate oil, and through refining to improve color and luster, smell, need improve stability.Divide according to boiling range scope, common are No. 90 solvent oils (boiling range 60 ~ 90 DEG C), No. 120 solvent oils (boiling range 90 ~ 120 DEG C), No. 150 solvent oils (boiling range 120 ~ 150 DEG C), No. 200 solvent oils (boiling range 140 ~ 200 DEG C), No. S-180 (boiling range 195 ~ 245 DEG C), No. S-1800 (boiling range 195 ~ 270 DEG C) etc.In general, boiling range higher than 150 DEG C be referred to as high boiling point solvent oil.Current domestic solvent oil market, the trade mark is numerous, and wherein varsol oil and benzene class (aromatic hydrocarbons) compound solvent oil respectively account for about half.
Heavy benzol, refer to acid wash processing crude benzol time from two benzene tower rectifying gas phase crude benzol time, the by product obtained at the bottom of tower, or hydrogenation method processing crude benzol prefractionation time, the by product obtained at the bottom of preliminary fractionator tower.Heavy benzol, primarily of the hydrocarbon compounds such as the aromatic hydroxy compounds such as dimethylbenzene, trimethylbenzene, naphthalene and high boiling point unsaturated compound vinylbenzene, coumarone and indenes and macromole sulfur-bearing, nitrogenous compound composition, has irritating smell.The component that wherein content is higher mainly contains indenes, coumarone, vinylbenzene, naphthalene, methylnaphthalene etc., and the content of naphthalene and methylnaphthalene accounts for 30%, and indenes content accounts for 25%.
Comprehensive utilization at present for heavy benzol mainly concentrates on hydrogenation and is separated two kinds of approach.Hydrogenation is about to the unsaturated double-bond hydrogenation except phenyl ring, removes the heteroatomss such as S, N, O simultaneously, makes its deodorizing of discoloring, and increase stability, hydrogenation difficulty is little; Separation is mainly physical means, is the chemical of solid by rectifying separation under going out the normal temperature such as naphthalene, methylnaphthalene.Comprehensive utilization report for heavy benzol resource mainly concentrates on the high added value industrial chemicals adopting various kinds physical separation method to extract different fractions, as: Chinese patent CN102617264A takes indenes, naphthalene, methylnaphthalene in low temperature side line rectifying separation heavy benzol; Chinese patent CN101143802A adopts rectifier unit to isolate indenes, naphthalene, methylnaphthalene.
Summary of the invention
The object of the invention is to provide a kind of heavy benzol lighting to produce the method for high boiling aromatic hydrocarbon solvent oil, directly can carry out hydrotreatment by counterweight benzene raw materials, promote the further utilization of coal tar.
Technical scheme of the present invention is: take heavy benzol as raw material, pre-hydrogenation, hydrocracking and hydrofining three reactors are passed through successively under catalyst action, again through rectifying separation, get the cut of 150 ~ 180 DEG C and the cut of 180 ~ 215 DEG C, be the high boiling aromatic hydrocarbon solvent oil meeting national standard.
In pre-hydrogenation step of the present invention, pre-hydrotreating reaction processing parameter is: temperature 220 ~ 300 DEG C, pressure 2 ~ 5 MPa, air speed 1 ~ 3.5 h
-1, hydrogen to oil volume ratio 200 ~ 800, sample bromine number < 3 g Br after hydrogenation
2/ 100g; Described pre-hydrogenator is fixed-bed reactor, is intended to the carbon carbon unsaturated double-bond hydrogenation beyond by phenyl ring in heavy benzol raw material, prevents oil product from high temperature gathering because unsaturated double bond is too high and causes catalyst deactivation with coking.
In scission reaction step of the present invention, scission reaction processing parameter is: temperature 350 ~ 430 DEG C, pressure 4 ~ 9 MPa, air speed 0.7 ~ 2.3 h
-1, hydrogen to oil volume ratio 300 ~ 1000; Described hydrocracking reactor is fixed-bed reactor, is intended to oil product lighting to generate, and reduces naphthalene nucleus aromaticity content, improves phenyl ring aromaticity content.
In refining reaction step of the present invention, refining reaction processing parameter is: temperature 200 ~ 320 DEG C, pressure 3 ~ 8 MPa, air speed 1 ~ 3.5 h
-1, hydrogen to oil volume ratio 200 ~ 800, described hydrofining reactor is fixed-bed reactor, is intended to the element hydrofining such as sulphur nitrogen in the oil product by hydrocracking and removes further, and improve east of oil.
The method of high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting of the present invention, and catalyst for pre-hydrogenation is identical with Hydrobon catalyst, and all adopt alchlor to be carrier, carrying active ingredients oxide compound is nickel oxide, molybdenum oxide, Tungsten oxide 99.999 and phosphorus oxide; Wherein, activeconstituents oxide compound gross weight is 20% ~ 60% of carrying alumina body weight, is preferably: 30% ~ 55%; The weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is: 10 ~ 30:50 ~ 85:3 ~ 20:0.5 ~ 8, preferably: 12 ~ 20:65 ~ 85:3 ~ 10:0.5 ~ 5.
Hydrocracking catalyst adopts sial complex carrier, and carrying active ingredients oxide compound is nickel oxide, Tungsten oxide 99.999 and phosphorus oxide; Wherein, activeconstituents oxide compound gross weight is 20% ~ 60% of sial complex carrier weight, is preferably: 25% ~ 45%; The weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is: 10 ~ 30:60 ~ 90:0.5 ~ 8, preferably: 15 ~ 25:65 ~ 85:0.5 ~ 5; In sial complex carrier, silicon oxide and alumina weight are than 20 ~ 70:30 ~ 80, preferably 50 ~ 70:30 ~ 50.
In preferred embodiment of the present invention, described catalyzer (comprising pre-hydrogenation, cracking and catalyst for refining), must through prevulcanized before participation reaction.Pre-vulcanization process is: be warming up to 150 DEG C under hydrogen atmosphere, pumps into dithiocarbonic anhydride activation oil, and the concentration of described dithiocarbonic anhydride activation oil is 1 ~ 3 wt%, is progressively warming up to 300 DEG C and activates, soak time 24 h.
In preferred embodiment of the present invention, described heavy benzene hydrogenation sample is pressed oil distillation through rectifying and is separated, and main products is for meeting high boiling aromatic hydrocarbons SA 1000 type solvent oil (boiling range 150 ~ 180 DEG C) and the SA 1500 type solvent oil (boiling range 180 ~ 215 DEG C) of GB (GB/T 29497-2013).Byproduct has: No. 90 solvent oils (boiling range 60 ~ 90 DEG C), No. 120 solvent oils (boiling range 90 ~ 120 DEG C) and xylol (boiling range 137 ~ 143 DEG C).Boiling point can be used as raw material higher than the cut of 215 DEG C, returns cracking reactor, recycled, improves aromatic solvent oil yield.
beneficial effect
The present invention take heavy benzol as raw material, pass through pre-hydrogenation, hydrocracking and hydrofining successively, be intended to produce mononuclear aromatics to the aromatic hydrocarbons of two or more ring through hydrocracking, effectively reduce the density of hydrogenation oil product, by oil distillation to the significantly movement of low temperature direction, there is obvious lighting effect.The direct counterweight benzene raw materials of the present invention carries out hydrotreatment, there is not loaded down with trivial details feed separation step, efficiency is improve while cost-saving, produce obtained high boiling aromatic hydrocarbon solvent oil and meet national standard, for promoting that the further utilization of coal tar is alleviated petroleum resources exhaustion and provided new effective way.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
Heavy benzol raw material passes through pre-hydrogenation, hydrocracking and hydrofining three reactors successively.The activeconstituents oxide compound gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A1 is 35% of carrying alumina body weight, and the weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is 15:70:10:5; The activeconstituents oxide compound gross weight of the B1 of hydrocracking catalyst is 30% of carrying alumina body weight, and the weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is 15:85:5, and in sial complex carrier, silicon oxide compares 5:5 with alumina weight.Pre-hydrogenator reaction conditions: temperature of reaction 250 DEG C, hydrogen pressure 4MPa, hydrogen to oil volume ratio 500:1, volume space velocity 3.0h
-1; Cracking reactor reaction conditions: temperature of reaction 380 DEG C, hydrogen pressure 8MPa, hydrogen to oil volume ratio 800:1, volume space velocity 2.0h
-1; Refining reaction device reaction conditions: temperature of reaction 300 DEG C, hydrogen pressure 5MPa, reaction hydrogen to oil volume ratio 300:1, volume space velocity 1.5h
-1.After three sections of hydrogenation, oil product cuts by boiling range the solvent oil product that 215 DEG C of front-end volatiles obtain different boiling range section, heavy constituent and rectifying tail oil after 215 DEG C.
embodiment 2
Heavy benzol raw material passes through pre-hydrogenation, hydrocracking and hydrofining three reactors successively.The activeconstituents oxide compound gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A2 is 50% of carrying alumina body weight, and the weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is 18:75:5:2; The activeconstituents oxide compound gross weight of the B2 of hydrocracking catalyst is 40% of carrying alumina body weight, and the weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is 20:75:5, and in sial complex carrier, silicon oxide compares 6:4 with alumina weight.Pre-hydrogenator reaction conditions: temperature of reaction 280 DEG C, hydrogen pressure 3MPa, hydrogen to oil volume ratio 300:1, volume space velocity 2.0h
-1; Cracking reactor reaction conditions: temperature of reaction 400 DEG C, hydrogen pressure 7MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.5h
-1; Refining reaction device reaction conditions: temperature of reaction 250 DEG C, hydrogen pressure 4MPa, reaction hydrogen to oil volume ratio 400:1, volume space velocity 2.0h
-1.After three sections of hydrogenation, oil product cuts by boiling range the solvent oil product that 215 DEG C of front-end volatiles obtain different boiling range section, heavy constituent and rectifying tail oil after 215 DEG C.
embodiment 3
Oil product after three sections of hydrogenation through rectifying separable go out 215 DEG C of front-end volatiles, heavy constituent and rectifying tail oil after 215 DEG C that do not steam.Rectifying tail oil and heavy benzol raw material are pressed the mixing of 1:1 volume ratio, pass through pre-hydrogenation, hydrocracking and hydrofining three reactors successively.The activeconstituents oxide compound gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A3 is 45% of carrying alumina body weight, and the weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is 10:80:6:4; The activeconstituents oxide compound gross weight of the B3 of hydrocracking catalyst is 60% of carrying alumina body weight, and the weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is 12:85:3, and in sial complex carrier, silicon oxide compares 7:3 with alumina weight.Pre-hydrogenator reaction conditions: temperature of reaction 220 DEG C, hydrogen pressure 3.5MPa, hydrogen to oil volume ratio 400:1, volume space velocity 3.5h
-1; Cracking reactor reaction conditions: temperature of reaction 360 DEG C, hydrogen pressure 6MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.2h
-1; Refining reaction device reaction conditions: temperature of reaction 330 DEG C, hydrogen pressure 6MPa, reaction hydrogen to oil volume ratio 500:1, volume space velocity 3.0h
-1.After three sections of hydrogenation, oil product cuts by boiling range the solvent oil product that 215 DEG C of front-end volatiles obtain different boiling range section, heavy constituent and rectifying tail oil after 215 DEG C.
In above embodiment, oil quality characteristic data before and after three sections of hydrogenation, refer to following table.
oil quality characteristic data before and after table 1. three sections of hydrogenation
In above embodiment, after three sections of hydrogenation, oil product obtains different boiling range section solvent oil and distillation tail oil through distillation, and yield ratio sees the following form.
table 2 different boiling range section product slates and density
As can be known from the above table, main products of the present invention is high boiling aromatic hydrocarbon solvent oil (150 ~ 180 DEG C and 180 ~ 215 DEG C of cuts) simultaneously by-product xylol (137 ~ 143 DEG C of cuts) and a small amount of 60 ~ 90 DEG C of cuts and 90 ~ 120 DEG C of cuts, following table lists 137 ~ 143 DEG C of cuts in above embodiment, 150 ~ 180 DEG C and 180 ~ 215 DEG C of cut solvent oil detailed analysis data, all meet corresponding Standard data, refer to following table 3.
table 3 the physical property of product and Standard data compare
Note: GB data
aadopt " 5 DEG C of xylol " data demand in " oil xylol " GB (GB/T 3407-2010); GB data
badopt " SA 1000 " data demand in " high boiling aromatic hydrocarbon solvent " GB (GB/T 29497-2013); GB data
cadopt " SA 1500 " data demand in " high boiling aromatic hydrocarbon solvent " GB (GB/T 29497-2013).
embodiment 4
Heavy benzol raw material catalyst for pre-hydrogenation A1, A2, A3 in embodiment 1-3 contrasts the catalytic performance of catalyst for pre-hydrogenation.Pre-hydrogenator reaction conditions: temperature of reaction 250 DEG C, hydrogen pressure 4MPa, hydrogen to oil volume ratio 500:1, volume space velocity 3.0h
-1; After hydrogenation, oil quality characteristic data, refer to following table.
table 4 is oil quality characteristic data after three kinds of catalyst for pre-hydrogenation hydrogenation
embodiment 5
The catalyst for pre-hydrogenation A2 of heavy benzol raw material in above-described embodiment carries out pre-hydrogenation, then B1, B2, B3 of hydrocracking catalyst contrasts the cracking performance of hydrocracking catalyst in above-described embodiment.Pre-hydrogenator reaction conditions: temperature of reaction 280 DEG C, hydrogen pressure 3MPa, hydrogen to oil volume ratio 300:1, volume space velocity 2.0h
-1; Cracking reactor reaction conditions: temperature of reaction 400 DEG C, hydrogen pressure 7MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.5h
-1; After hydrogenation, oil quality characteristic data, refer to following table.
table 5 is oil quality characteristic data after three kinds of catalyst for cracking hydrogenation
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (8)
1. the method for a heavy benzol lighting production high boiling aromatic hydrocarbon solvent oil, it is characterized in that: take heavy benzol as raw material, pre-hydrogenation, hydrocracking and hydrofining three reactors are passed through successively under catalyst action, again through rectifying separation, after getting the cut of the cut of 150 ~ 180 DEG C or 180 ~ 215 DEG C and get final product.
2. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 1, it is characterized in that: in described pre-hydrogenation step, pre-hydrotreating reaction processing parameter is: temperature 220 ~ 300 DEG C, pressure 2 ~ 5 MPa, air speed 1 ~ 3.5h
-1, hydrogen to oil volume ratio 200 ~ 800, sample bromine number < 3gBr after hydrogenation
2/ 100g; In described scission reaction step, scission reaction processing parameter is: temperature 350 ~ 430 DEG C, pressure 4 ~ 9MPa, air speed 0.7 ~ 2.3h-1, hydrogen to oil volume ratio 300 ~ 1000; In described refining reaction step, refining reaction processing parameter is: temperature 200 ~ 320 DEG C, pressure 3 ~ 8MPa, air speed 1 ~ 3.5h-1, hydrogen to oil volume ratio 200 ~ 800; Described reactor is fixed-bed reactor.
3. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 1, it is characterized in that: described catalyst for pre-hydrogenation is identical with Hydrobon catalyst, all adopt alchlor to be carrier, carrying active ingredients oxide compound is nickel oxide, molybdenum oxide, Tungsten oxide 99.999 and phosphorus oxide; Wherein activeconstituents oxide compound gross weight is 20% ~ 60% of carrying alumina body weight, and the weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is: 10 ~ 30:50 ~ 85:3 ~ 20:0.5 ~ 8.
4. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 3, it is characterized in that: described catalyst for pre-hydrogenation and Hydrobon catalyst activeconstituents oxide compound gross weight are 30% ~ 55% of carrying alumina body weight; The weight ratio of nickel oxide, molybdenum oxide, Tungsten oxide 99.999, phosphorus oxide is 12 ~ 20:65 ~ 85:3 ~ 10:0.5 ~ 5.
5. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 1, it is characterized in that: described hydrocracking catalyst adopts sial complex carrier, and carrying active ingredients oxide compound is nickel oxide, Tungsten oxide 99.999 and phosphorus oxide; Wherein, activeconstituents oxide compound gross weight is 20% ~ 60% of sial complex carrier weight; The weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is: 10 ~ 30:60 ~ 90:0.5 ~ 8; In sial complex carrier, silicon oxide and alumina weight are than 20 ~ 70:30 ~ 80.
6. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 5, it is characterized in that: described hydrocracking catalyst activeconstituents oxide compound gross weight is 25% ~ 45% of sial complex carrier weight; The weight ratio of nickel oxide, Tungsten oxide 99.999, phosphorus oxide is: 15 ~ 25:65 ~ 85:0.5 ~ 5; In sial complex carrier, silicon oxide and alumina weight are than 50 ~ 70:30 ~ 50.
7. produce the method for high boiling aromatic hydrocarbon solvent oil according to the arbitrary described heavy benzol lighting of claim 1-6, it is characterized in that: described catalyzer, must through prevulcanized before participation reaction.
8. the method for high boiling aromatic hydrocarbon solvent oil is produced in heavy benzol lighting according to claim 7, it is characterized in that: described pre-vulcanization process is: under hydrogen atmosphere, be warming up to 150 DEG C, pump into dithiocarbonic anhydride activation oil, the concentration of described dithiocarbonic anhydride activation oil is 1 ~ 3wt%, progressively be warming up to 300 DEG C to activate, soak time 24h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105176583A (en) * | 2015-10-12 | 2015-12-23 | 苏州常实工业设备有限公司 | Catalytic reforming preparation method of high performance solvent oil |
| CN108855163A (en) * | 2017-05-16 | 2018-11-23 | 江苏华伦化工有限公司 | A kind of ten tail oil catalyst for cracking of reformation carbon and its preparation and application |
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| CN101712888A (en) * | 2009-11-26 | 2010-05-26 | 湖南长岭石化科技开发有限公司 | Hydrofining technology of heavy benzol |
| CN103520945A (en) * | 2012-07-04 | 2014-01-22 | 天津大学 | Device and method for refining crude benzene hydrogenation product |
| CN104152179A (en) * | 2014-09-01 | 2014-11-19 | 江苏联东化工股份有限公司 | Production method of high-boiling-point aromatic solvent oil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5763721A (en) * | 1996-12-12 | 1998-06-09 | Phillips Petroleum Company | Hydrodealkylation of C9+ aromatic compounds |
| CN101712888A (en) * | 2009-11-26 | 2010-05-26 | 湖南长岭石化科技开发有限公司 | Hydrofining technology of heavy benzol |
| CN103520945A (en) * | 2012-07-04 | 2014-01-22 | 天津大学 | Device and method for refining crude benzene hydrogenation product |
| CN104152179A (en) * | 2014-09-01 | 2014-11-19 | 江苏联东化工股份有限公司 | Production method of high-boiling-point aromatic solvent oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105176583A (en) * | 2015-10-12 | 2015-12-23 | 苏州常实工业设备有限公司 | Catalytic reforming preparation method of high performance solvent oil |
| CN108855163A (en) * | 2017-05-16 | 2018-11-23 | 江苏华伦化工有限公司 | A kind of ten tail oil catalyst for cracking of reformation carbon and its preparation and application |
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