CN104927917B - A kind of heavy benzol lighting produces the method for high boiling aromatic hydrocarbon solvent oil - Google Patents
A kind of heavy benzol lighting produces the method for high boiling aromatic hydrocarbon solvent oil Download PDFInfo
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Abstract
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 heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil. The present invention, with heavy benzol for raw material, sequentially passes through pre-hydrogenation, hydrocracking and three reactors of hydrofinishing under catalyst action, separates then through rectification, takes the fraction of 150��180 DEG C and namely the fraction of 180��215 DEG C obtains the solvent naphtha product of corresponding boiling range section. It is contemplated that the hydrogenated cracking of aromatic hydrocarbons of two or more ring is produced mononuclear aromatics, effectively reduce the density of hydrogenation oil product, oil distillation is significantly mobile to low temperature direction, there is obvious lighting effect. The direct counterweight benzene raw materials of the present invention carries out hydrotreatment, is absent from loaded down with trivial details feed separation step, saves cost and reduces energy consumption, and prepared high boiling aromatic hydrocarbon solvent oil meets national standard. The present invention is for promoting that the further utilization of coal tar alleviates the effective way that petroleum resources exhaustion provides new.
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 heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil.
Background technology
As one of main oil product, solvent naphtha is together with gasoline, kerosene, diesel oil, lubricating oil and is called the big class oil product of China five. Solvent naphtha has a wide range of applications in industries such as medicine, chemical industry, macromolecular material, rubber and paint. At present, the primary raw material that solvent naphtha produces has three sources: crude oil straight-run, and catalytic reforming is raffinated oil and condensate, and need to pass through refining to improve color and luster, abnormal smells from the patient, improves stability. Divide according to boiling range scope, common are No. 90 solvent naphthas (boiling range 60��90 DEG C), No. 120 solvent naphthas (boiling range 90��120 DEG C), No. 150 solvent naphthas (boiling range 120��150 DEG C), No. 200 solvent naphthas (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 naphtha 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 column rectification gas phase crude benzol time, the by-product obtained at the bottom of tower, or hydrogenation method processing crude benzol prefractionation time, from the by-product obtained at the bottom of prefractionator tower. Heavy benzol is mainly made up of the hydrocarbon compounds such as the aromatic compounds such as dimethylbenzene, trimethylbenzene, naphthalene and high boiling point unsaturated compound styrene, coumarone and indenes and macromole sulfur-bearing, nitrogen-containing compound, has penetrating odor. The component that wherein content is higher mainly has indenes, coumarone, styrene, naphthalene, methyl naphthalene etc., and the content of naphthalene and methyl naphthalene accounts for 30%, and indenes content accounts for 25%.
Comprehensive utilization currently for heavy benzol is concentrated mainly on hydrogenation and separates two kinds of approach. Hydrogenation is about to the unsaturated double-bond hydrogenation except phenyl ring, removes the hetero atoms such as S, N, O so that it is deodorization of discoloring simultaneously, increases stability, and hydrogenation difficulty is little;Separation is mainly physical means, is isolated under the room temperature such as naphthalene, methyl naphthalene as the chemicals of solid by rectification. Comprehensive utilization report for heavy benzol resource is concentrated mainly on the high added value industrial chemicals adopting various kinds physical separation method to extract different fractions, as: Chinese patent CN102617264A takes indenes, naphthalene, methyl naphthalene in low temperature side line rectification separation heavy benzol; Chinese patent CN101143802A adopts rectifier unit to isolate indenes, naphthalene, methyl naphthalene.
Summary of the invention
A kind of method that present invention aim at providing heavy benzol lighting to produce high boiling aromatic hydrocarbon solvent oil, it is possible to directly counterweight benzene raw materials carries out hydrotreatment, promotes the further utilization of coal tar.
The technical scheme is that with heavy benzol for raw material, pre-hydrogenation, hydrocracking and three reactors of hydrofinishing are sequentially passed through under catalyst action, separate then through rectification, take the fraction of 150��180 DEG C and the fraction 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 technological parameter is: temperature 220 ~ 300 DEG C, pressure 2 ~ 5MPa, air speed 1 ~ 3.5h-1, hydrogen to oil volume ratio 200 ~ 800, sample bromine number < 3gBr after hydrogenation2/ 100g; Described pre-hydrogenator is fixed bed reactors, it is intended to be hydrogenated with by the carbon carbon unsaturated double-bond beyond phenyl ring in heavy benzol raw material, it is prevented that oil product is because unsaturated double bond is too high at high temperature poly-and coking causes catalysqt deactivation.
In cracking reaction step of the present invention, cracking reaction technological parameter is: temperature 350 ~ 430 DEG C, pressure 4 ~ 9MPa, air speed 0.7 ~ 2.3h-1, hydrogen to oil volume ratio 300 ~ 1000; Described hydrocracking reactor is fixed bed reactors, it is intended to oil product lighting generated, and reduces naphthalene nucleus arene content, improves phenyl ring arene content.
In refining reaction step of the present invention, refining reaction technological parameter is: temperature 200 ~ 320 DEG C, pressure 3 ~ 8MPa, air speed 1 ~ 3.5h-1, hydrogen to oil volume ratio 200 ~ 800, described hydrofining reactor is fixed bed reactors, it is intended to the element hydrofinishings such as sulfur nitrogen in the oil product of hydrocracking is removed further, and improves east of oil.
Heavy benzol lighting of the present invention produces the method for high boiling aromatic hydrocarbon solvent oil, and catalyst for pre-hydrogenation is identical with Hydrobon catalyst, and all adopting alchlor is carrier, and carrying active ingredients oxide is nickel oxide, molybdenum oxide, tungsten oxide and phosphorous oxide; Wherein, active component oxide gross weight is the 20%��60% of carrying alumina body weight, it is preferred to: 30%��55%; Nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be: 10��30:50��85:3��20:0.5��8, it is preferable that: 12��20:65��85:3��10:0.5��5.
Hydrocracking catalyst adopts sial complex carrier, and carrying active ingredients oxide is nickel oxide, tungsten oxide and phosphorous oxide; Wherein, active component oxide gross weight is the 20%��60% of sial complex carrier weight, it is preferred to: 25%��45%; Nickel oxide, tungsten oxide, phosphorous oxide weight ratio be: 10��30:60��90:0.5��8, it is preferable that: 15��25:65��85:0.5��5; In sial complex carrier, silicon oxide and alumina weight are than 20��70:30��80, it is preferable that 50��70:30��50.
In the preferred embodiment of the present invention, described catalyst (includes pre-hydrogenation, cracking and catalyst for refining) before participating in reaction, must through presulfurization. Pre-vulcanization process is: be warming up to 150 DEG C under hydrogen atmosphere, pumps into Carbon bisulfide activation oil, and the concentration of described Carbon bisulfide activation oil is 1��3wt%, is progressively warming up to 300 DEG C and activates, soak time 24h.
In the preferred embodiment of the present invention, described heavy benzene hydrogenation sample is pressed oil distillation through rectification and is separated, and major product is meet high boiling aromatic hydrocarbons SA1000 type solvent naphtha (boiling range 150��180 DEG C) and the SA1500 type solvent naphtha (boiling range 180��215 DEG C) of GB (GB/T29497-2013). Side-product has: No. 90 solvent naphthas (boiling range 60��90 DEG C), No. 120 solvent naphthas (boiling range 90��120 DEG C) and mixed xylenes (boiling range 137��143 DEG C). The boiling point fraction higher than 215 DEG C as raw material, can return cracking reactor, recycled, improve aromatic solvent oil yield.
Beneficial effect
The present invention is with heavy benzol for raw material, sequentially pass through pre-hydrogenation, hydrocracking and hydrofinishing, it is intended to the hydrogenated cracking of aromatic hydrocarbons of two or more ring is produced mononuclear aromatics, effectively reduces the density of hydrogenation oil product, oil distillation is significantly mobile to low temperature direction, there is obvious lighting effect. The direct counterweight benzene raw materials of the present invention carries out hydrotreatment, it is absent from loaded down with trivial details feed separation step, efficiency is improve while saving cost, produced the high boiling aromatic hydrocarbon solvent oil prepared and met national standard, for promoting that the further utilization of coal tar alleviates the effective way that petroleum resources exhaustion provides new.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, so that those skilled in the art are more fully understood that the present invention, but the invention is not limited in following example.
Embodiment 1
Heavy benzol raw material sequentially passes through pre-hydrogenation, hydrocracking and three reactors of hydrofinishing. The active component oxide gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A1 is the 35% of carrying alumina body weight, nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be 15:70:10:5; The active component oxide gross weight of the B1 of hydrocracking catalyst is the 30% of carrying alumina body weight, nickel oxide, tungsten oxide, phosphorous oxide weight ratio be 15:85:5, in sial complex carrier, silicon oxide compares 5:5 with alumina weight. Pre-hydrogenator reaction condition: reaction temperature 250 DEG C, hydrogen pressure 4MPa, hydrogen to oil volume ratio 500:1, volume space velocity 3.0h-1; Cracking reactor reaction condition: reaction temperature 380 DEG C, hydrogen pressure 8MPa, hydrogen to oil volume ratio 800:1, volume space velocity 2.0h-1; Refining reaction device reaction condition: reaction temperature 300 DEG C, hydrogen pressure 5MPa, reaction hydrogen to oil volume ratio 300:1, volume space velocity 1.5h-1. After three sections are hydrogenated with, oil product is cut 215 DEG C of front-end volatiles by boiling range and is obtained the solvent naphtha product of different boiling range section, heavy constituent and rectification tail oil after 215 DEG C.
Embodiment 2
Heavy benzol raw material sequentially passes through pre-hydrogenation, hydrocracking and three reactors of hydrofinishing. The active component oxide gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A2 is the 50% of carrying alumina body weight, nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be 18:75:5:2; The active component oxide gross weight of the B2 of hydrocracking catalyst is the 40% of carrying alumina body weight, nickel oxide, tungsten oxide, phosphorous oxide weight ratio be 20:75:5, in sial complex carrier, silicon oxide compares 6:4 with alumina weight. Pre-hydrogenator reaction condition: reaction temperature 280 DEG C, hydrogen pressure 3MPa, hydrogen to oil volume ratio 300:1, volume space velocity 2.0h-1; Cracking reactor reaction condition: reaction temperature 400 DEG C, hydrogen pressure 7MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.5h-1; Refining reaction device reaction condition: reaction temperature 250 DEG C, hydrogen pressure 4MPa, reaction hydrogen to oil volume ratio 400:1, volume space velocity 2.0h-1.After three sections are hydrogenated with, oil product is cut 215 DEG C of front-end volatiles by boiling range and is obtained the solvent naphtha product of different boiling range section, heavy constituent and rectification tail oil after 215 DEG C.
Embodiment 3
Oil product after three sections are hydrogenated with may separate out 215 DEG C of front-end volatiles through rectification, heavy constituent and rectification tail oil after 215 DEG C not steamed. Rectification tail oil and heavy benzol raw material are pressed the mixing of 1:1 volume ratio, sequentially passes through pre-hydrogenation, hydrocracking and three reactors of hydrofinishing. The active component oxide gross weight of catalyst for pre-hydrogenation and Hydrobon catalyst A3 is the 45% of carrying alumina body weight, nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be 10:80:6:4; The active component oxide gross weight of the B3 of hydrocracking catalyst is the 60% of carrying alumina body weight, nickel oxide, tungsten oxide, phosphorous oxide weight ratio be 12:85:3, in sial complex carrier, silicon oxide compares 7:3 with alumina weight. Pre-hydrogenator reaction condition: reaction temperature 220 DEG C, hydrogen pressure 3.5MPa, hydrogen to oil volume ratio 400:1, volume space velocity 3.5h-1; Cracking reactor reaction condition: reaction temperature 360 DEG C, hydrogen pressure 6MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.2h-1; Refining reaction device reaction condition: reaction temperature 330 DEG C, hydrogen pressure 6MPa, reaction hydrogen to oil volume ratio 500:1, volume space velocity 3.0h-1. After three sections are hydrogenated with, oil product is cut 215 DEG C of front-end volatiles by boiling range and is obtained the solvent naphtha product of different boiling range section, heavy constituent and rectification tail oil after 215 DEG C.
In above example, oil quality characteristic data before and after three sections of hydrogenation, refer to following table.
Oil quality characteristic data before and after 1. 3 sections of table hydrogenation
In above example, after three sections of hydrogenation, oil product obtains different boiling range section solvent naphtha and distillation tail oil through distillation, and yield ratio is shown in following table.
The different boiling range section product slates of table 2 and density
As can be known from the above table, by-product mixed xylenes (137��143 DEG C of fractions) and a small amount of 60��90 DEG C of fractions and 90��120 DEG C of fractions while that major product of the present invention being high boiling aromatic hydrocarbon solvent oil (150��180 DEG C and 180��215 DEG C of fractions), following table lists 137��143 DEG C of fractions in above example, 150��180 DEG C and 180��215 DEG C of fraction solvent naphtha labor data, all meet corresponding Standard data, refer to table 3 below.
Table 3 the physical property of product and Standard data compare
Note: GB dataaAdopt " 5 DEG C of mixed xylenes " data demand in " oil mixed xylenes " GB (GB/T3407-2010); GB databAdopt " SA1000 " data demand in " high boiling aromatic hydrocarbon solvent " GB (GB/T29497-2013); GB datacAdopt " SA1500 " data demand in " high boiling aromatic hydrocarbon solvent " GB (GB/T29497-2013).
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 condition: reaction temperature 250 DEG C, hydrogen pressure 4MPa, hydrogen to oil volume ratio 500:1, volume space velocity 3.0h-1; Oil quality characteristic data after hydrogenation, refer to following table.
Table 4 is oil quality characteristic data after three kinds of catalyst for pre-hydrogenation hydrogenation
Embodiment 5
Heavy benzol raw material catalyst for pre-hydrogenation A2 in above-described embodiment is hydrogenated with in advance, contrasts the cracking performance of hydrocracking catalyst then through B1, B2, B3 of hydrocracking catalyst in above-described embodiment. Pre-hydrogenator reaction condition: reaction temperature 280 DEG C, hydrogen pressure 3MPa, hydrogen to oil volume ratio 300:1, volume space velocity 2.0h-1;Cracking reactor reaction condition: reaction temperature 400 DEG C, hydrogen pressure 7MPa, hydrogen to oil volume ratio 500:1, volume space velocity 1.5h-1; Oil quality characteristic data after hydrogenation, 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 equivalent structure utilizing description of the present invention to make or equivalence flow process conversion, or directly or indirectly it is used in other relevant technical fields, all in like manner include in the scope of patent protection of the present invention.
Claims (8)
1. the method that a heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil, it is characterized in that, with heavy benzol for raw material, pre-hydrogenation, hydrocracking and three reactors of hydrofinishing are sequentially passed through under catalyst action, separate then through rectification, after taking the fraction of 150��180 DEG C or the fraction of 180��215 DEG C and get final product.
2. the method that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 1, it is characterised in that:
In described pre-hydrogenation step, pre-hydrotreating reaction technological parameter is: temperature 220 ~ 300 DEG C, pressure 2 ~ 5MPa, air speed 1 ~ 3.5h-1, hydrogen to oil volume ratio 200 ~ 800, sample bromine number < 3gBr after hydrogenation2/ 100g;
In described cracking reaction step, cracking reaction technological 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 technological 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 reactors.
3. the method that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 1, it is characterized in that, described catalyst for pre-hydrogenation is identical with Hydrobon catalyst, and all adopting aluminium oxide is carrier, and carrying active ingredients oxide is nickel oxide, molybdenum oxide, tungsten oxide and phosphorous oxide; Wherein active component oxide gross weight is the 20%��60% of carrying alumina body weight, nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be: 10��30:50��85:3��20:0.5��8.
4. the method that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 3, it is characterised in that described catalyst for pre-hydrogenation and Hydrobon catalyst active component oxide gross weight are the 30%��55% of carrying alumina body weight; Nickel oxide, molybdenum oxide, tungsten oxide, phosphorous oxide weight ratio be 12��20:65��85:3��10:0.5��5.
5. the method that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 1, it is characterised in that described hydrocracking catalyst adopts sial complex carrier, and carrying active ingredients oxide is nickel oxide, tungsten oxide and phosphorous oxide; Wherein, active component oxide gross weight is the 20%��60% of sial complex carrier weight; Nickel oxide, tungsten oxide, phosphorous oxide weight ratio be: 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 that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 5, it is characterised in that described hydrocracking catalyst active component oxide gross weight is the 25%��45% of sial complex carrier weight; Nickel oxide, tungsten oxide, phosphorous oxide weight ratio be: 15��25:65��85:0.5��5; In sial complex carrier, silicon oxide and alumina weight are than 50��70:30��50.
7. the method producing high boiling aromatic hydrocarbon solvent oil according to the arbitrary described heavy benzol lighting of claim 1-6, it is characterised in that described catalyst, must through presulfurization before participating in reaction.
8. the method that heavy benzol lighting produces high boiling aromatic hydrocarbon solvent oil according to claim 7, it is characterized in that, described pre-vulcanization process is: be warming up to 150 DEG C under hydrogen atmosphere, pump into Carbon bisulfide activation oil, the concentration of described Carbon bisulfide activation oil is 1��3wt%, progressively it is warming up to 300 DEG C to activate, soak time 24h.
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| CN101712888B (en) * | 2009-11-26 | 2012-09-12 | 湖南长岭石化科技开发有限公司 | Hydrofining technology of heavy benzol |
| CN103520945B (en) * | 2012-07-04 | 2016-05-25 | 天津大学 | The refining plant of crude benzole hydrogenation product and method |
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