CN116640603A - Method for refining crude benzene and preparing byproduct high-boiling-point solvent oil - Google Patents
Method for refining crude benzene and preparing byproduct high-boiling-point solvent oil Download PDFInfo
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- CN116640603A CN116640603A CN202211278531.8A CN202211278531A CN116640603A CN 116640603 A CN116640603 A CN 116640603A CN 202211278531 A CN202211278531 A CN 202211278531A CN 116640603 A CN116640603 A CN 116640603A
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 title claims abstract description 271
- 239000002904 solvent Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007670 refining Methods 0.000 title claims abstract description 17
- 239000006227 byproduct Substances 0.000 title claims abstract description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000009835 boiling Methods 0.000 claims abstract description 41
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000008096 xylene Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims description 37
- 238000005984 hydrogenation reaction Methods 0.000 claims description 37
- 229910003294 NiMo Inorganic materials 0.000 claims description 26
- 238000000605 extraction Methods 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 35
- 239000000047 product Substances 0.000 description 14
- 238000004939 coking Methods 0.000 description 10
- 238000012856 packing Methods 0.000 description 6
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 5
- 238000005194 fractionation Methods 0.000 description 5
- 238000003889 chemical engineering Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- -1 xylene aromatic compounds Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention belongs to the technical field of crude benzene refining, and provides a method for refining crude benzene and by-producing high-boiling-point solvent oil, which comprises the following steps: firstly, preheating crude benzene, entering a prefractionator, and removing low boiling point compounds and heavy benzene; and (3) hydrofining reaction, wherein the refined materials after treatment enter two rectifying towers to produce high-purity benzene, high-purity toluene, dimethylbenzene and byproduct high-boiling solvent oil. On the premise of ensuring that the yields and the quality of benzene, toluene and xylene are not reduced, the invention optimizes the temperature of the tower kettle of the prefractionator and the side line of the toluene tower to extract the xylene, and the byproduct solvent oil with high boiling point in the tower kettle has the advantages of simple process, stable operation, low production cost, aromatic hydrocarbon recovery rate, no need of adding a separation device such as a rectifying tower and the like, thereby increasing the economic benefit and the social benefit of enterprises.
Description
Technical Field
The invention belongs to the technical field of crude benzene refining, and particularly relates to a method for refining crude benzene and preparing byproduct high-boiling-point solvent oil.
Background
The coking crude benzene is a light distillate oil recovered from crude gas produced in the coking process, wherein the content of benzene, toluene and xylene aromatic compounds can reach more than 90%, the content of high-boiling-point solvent oil (the main component is C9 compounds) is about 1%, and the coking crude benzene is widely applied to fine chemical industry and organic synthesis industry, and the coking crude benzene reaches 428 ten thousand tons in 2017 according to statistics, so the coking crude benzene is one of important sources of the high-boiling-point solvent oil. Under the premise of ensuring the production of high-quality benzene, toluene and xylene by technical transformation in the traditional coking crude benzene hydrofining process, large-scale separation equipment such as a rectifying tower and the like are not added, the byproduct of high-boiling-point solvent oil is realized, the recycling utilization of coking crude benzene is improved, and the economic benefit of enterprises is improved.
The prefractionation process of traditional coking crude benzene hydrofining is that the coking crude benzene is preheated to 65-72 ℃ by a heat exchanger and enters a prefractionation tower, the low boiling point component and heavy benzene are removed in the process, and the sulfur-containing and nitrogen-containing compounds are converted into H by hydrofining reaction 2 S、NH 3 The refined fraction enters a first rectifying tower and a second rectifying tower to obtain high-purity benzene, toluene and xylene. In order to ensure the quality of the dimethylbenzene, the high-boiling solvent oil is cut into the heavy benzene by strictly controlling the technological parameters of the prefractionator, so that the resource waste is caused. In conclusion, the design of the byproduct high-boiling-point solvent oil in the crude benzene refining process has important significance.
CN103013560a proposes that the product of coking crude benzene after heavy benzene removal is hydrofined and rectified to obtain benzene, toluene, xylene, high boiling point solvent oil at 150-175 ℃ and 180-200 ℃, the separation unit needs at least 4-5 rectifying towers, the traditional crude benzene refining enterprise generally only has 2 rectifying towers for separating benzene, toluene and xylene, and the rectifying towers are added for byproduct high boiling point solvent oil, so that not only field and a great deal of funds are needed, but also evaluation such as environment and safety is needed; CN103520945 proposes a crude benzene hydrofining device and method, and the hydrogenation product is separated by rectification to obtain benzene, toluene and xylene, without byproduct solvent. In conclusion, the technology for developing the byproduct high-boiling-point solvent oil in the crude benzene refining process without adding new separation equipment is simple in process, and has higher economic and social benefits.
Disclosure of Invention
The invention provides the method for preparing the byproduct high-boiling solvent oil, which has the advantages of simple process, stable operation, low production cost, high aromatic recovery rate, no need of adding a separating device such as a rectifying tower and the like.
A method for refining crude benzene and preparing byproduct high-boiling solvent oil comprises the following specific steps:
(1) Prefractionation of crude benzene:
prefractionating the crude benzene raw material to remove low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
mixing the prefractionated material with hydrogen, heating and pressurizing, introducing into a first hydrogenation reactor and a second hydrogenation reactor, respectively carrying out unsaturated component hydrogenation reaction, hydrodesulfurization and hydrodenitrogenation reaction, and removing sulfur-containing and nitrogen-containing mixtures, thereby producing high-quality aromatic compounds such as benzene, toluene and xylene.
(3) And (3) rectifying and separating:
and (3) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower and a second rectifying tower, high-purity benzene and toluene are respectively extracted from the tops of the first rectifying tower and the second rectifying tower, a side line extraction process is adopted, and xylene and high-boiling solvent oil are respectively extracted from the side line and the tower bottom of the second rectifying tower.
As one of the preferred modes of the present invention, in the step (1), the prefractionation process parameters are as follows: the feeding temperature of crude benzene is 69-72 ℃; the temperature of the top of the prefractionation tower is 67-68 ℃ and the pressure is-52 to-55 kPa; the temperature of the tower bottom of the prefractionation tower is 160-175 ℃ and the pressure is-30 to-40 kPa;
in the step (2), a first hydrogenation reactor adopts a NiMo catalyst, a small amount of NiMo catalyst is loaded in a second hydrogenation reactor to be mixed with a traditional hydrofining catalyst CoMo catalyst, and the loading ratio of the NiMo catalyst to the CoMo catalyst is 1: 19-1: 3, wherein NiMo catalyst MoO 3 The content is 8-12 wt%.
As one of the preferable modes of the invention, in the step (3), the temperature of the tower bottom of the second rectifying tower is 150-165 ℃, the pressure is 45-60 kPa, the side line extraction positions are 55-62, and the temperature is 143-146 ℃.
Compared with the prior art, the invention has the advantages that:
according to the invention, by increasing the temperature of the bottom of the prefractionation tower, more aromatic compounds in the crude benzene raw material are distilled out, partial catalyst of the second hydrogenation reactor is optimized, hydrogenation, desulfurization and denitrification performance of the catalyst are improved, the side line of the second rectification tower is additionally arranged, and separation of high boiling point solvent oil is realized, and the above three are coupled, so that the operation elasticity of the prefractionation tower for temperature control is enhanced, the utilization rate of heavy components in the raw material is improved, and the economic and social benefits of enterprises are increased.
The invention has the following specific advantages:
(1) The invention improves the temperature of the tower kettle of the prefractionation tower, not only is beneficial to distilling benzene, toluene and xylene aromatic compounds in the crude benzene raw material, but also evaporates the high boiling point solvent oil mainly comprising C9 components, thereby laying a foundation for recycling heavy benzene;
(2) According to the invention, part of NiMo catalyst is mixed in the second hydrogenation reactor, so that the hydrodenitrogenation performance of the reaction unit is improved, and the production of colorless or pale yellow solvent with low nitrogen content and higher stability is facilitated;
(3) According to the invention, a side line extraction facility is additionally arranged on the second rectifying tower, so that the separation of three components (toluene, dimethylbenzene and high boiling point solvent oil) in one tower is realized on the premise of not increasing large equipment of the rectifying tower, and the economic benefit of enterprises is increased;
(4) The invention increases the temperature of the pre-distillation tower kettle, optimizes partial catalyst of the second hydrogenation reactor and adds coupling to the side line of the second distillation tower. The traditional crude benzene prefractionation operation changes the fractionation temperature point of the crude benzene prefractionation operation into a fractionation temperature interval by strictly controlling the fractionation temperature, the fractionation temperature is lower, the recovery rate of the 'triphenyl', the fractionation temperature is higher, and the heavy components influence the purity of the dimethylbenzene.
Drawings
FIG. 1 is a process flow diagram of a byproduct high boiling point solvent oil from crude benzene refining; wherein, the device comprises a 1-prefractionator, a 2-stripping section, a 3-tower kettle, a 4-rectifying tower, a 5-stripping section and a 6-side line extraction section; 101-a prefractionator, 102-a first hydrogenation reactor, 103-a second hydrogenation reactor, 104-a first rectifying tower and 105-a second rectifying tower; 11-crude benzene, 12-prefractionation tower top product, 13-prefractionation tower bottom product (heavy benzene), 14-refined product, 15-benzene, 16-first rectification tower bottom product, 17-toluene, 18-dimethylbenzene and 19-high boiling solvent oil;
FIG. 2 is the effect of mass fraction of p-toluene, xylenes and C9 component high boiling solvent oils in the theoretical plate number of the second rectification column.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Example 1
As shown in fig. 1, the method for refining crude benzene and by-producing high boiling solvent oil in this embodiment comprises the following specific steps:
(1) Prefractionation of crude benzene:
pre-fractionating raw material of crude benzene 11, wherein the temperature of a tower kettle 3 is 160 ℃, the pressure of the tower kettle 3 is-30 kPa, and removing low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
by increasing the temperature of the pre-distillation tower kettle 3, the content of 'triphenyl' (benzene, toluene and xylene) in the product after pre-distillation treatment is slightly increased, and the content of high-boiling solvent oil taking C9 components as main fractions is increased, but the mass fraction of the nitrogen-containing compounds contained in the product is increased. Mixing the prefractionated material with hydrogen, heating and pressurizing, introducing into a first hydrogenation reactor 102 and a second hydrogenation reactor 103, wherein the first hydrogenation reactor 102 adopts a NiMo catalyst, the NiMo catalyst is M8-21, and the filling density is 0.7g/cm 3 To improve the hydrodenitrogenation performance of the hydrofinishing, the conventional part of the CoMo catalyst is replaced by NiMo catalysis in the second hydrogenation reactor 103, wherein the mass ratio of NiMo to CoMo is 1:19, the CoMo catalyst is M8-12, contains 5% wtnio, contains 12% wtmoo 3 Packing density of 0.75g/cm 3 The reaction temperature and the reaction pressure are kept unchanged.
(3) And (3) rectifying and separating:
and (2) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower 104 and a second rectifying tower 105, high-purity benzene and toluene 17 are respectively extracted from the tops of the first rectifying tower 104 and the second rectifying tower 105, a side line extraction process is adopted, a side line extraction port is positioned on a 62 th column plate, the temperature of the column plate is controlled to be 146 ℃, the temperature of a column bottom is controlled to be 150 ℃, the pressure of the column bottom is 45kPa, and xylene 18 and high-boiling-point solvent oil 19 are respectively extracted from the side line and the column bottom of the second rectifying tower.
Example 2
As shown in fig. 1, the method for refining crude benzene and by-producing high boiling solvent oil in this embodiment comprises the following specific steps:
(1) Prefractionation of crude benzene:
pre-fractionating raw material of crude benzene 11, wherein the temperature of a tower kettle is 164 ℃, the pressure of the tower kettle is-35 kPa, and removing low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
by increasing the temperature of the pre-distillation tower kettle 3, the content of 'triphenyl' (benzene, toluene and xylene) in the product after pre-distillation treatment is slightly increased, and the content of high-boiling solvent oil taking C9 components as main fractions is increased, but the mass fraction of the nitrogen-containing compounds contained in the product is increased. Mixing the prefractionated material with hydrogen, heating and pressurizing, and introducing into a first hydrogenation reactor 102 and a second hydrogenation reactor 103, wherein the first hydrogenation reactor adopts a NiMo catalyst, the NiMo catalyst is M8-21, and the packing density is 0.7g/cm 3 To improve the hydrodenitrogenation performance of the hydrofining, the conventional part of the CoMo catalyst is replaced by NiMo catalyst in the second hydrogenation reactor 103, wherein the mass ratio of NiMo to CoMo is 1:9, and the NiMo catalyst CNBR-01 is manufactured by southwest chemical engineering institute of design, inc., contains 5% wtNiO and 8% wtMoO 3 Packing density of 0.75g/cm 3 Reaction temperature the reaction pressure remained unchanged.
(3) And (3) rectifying and separating:
and (2) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower 104 and a second rectifying tower 105, high-purity benzene and toluene are respectively extracted from the tops of the first rectifying tower 104 and the second rectifying tower 105, a side line extraction process is adopted, a side line extraction port is positioned on a 60 th column plate, the temperature of the column plate is controlled to 145 ℃, the temperature of a column bottom is 158 ℃, the pressure of the column bottom is 50kPa, and xylene 18 and high-boiling solvent oil 19 are respectively extracted from the side line and the column bottom of the second rectifying tower.
Example 3
As shown in fig. 1, the method for refining crude benzene and by-producing high boiling solvent oil in this embodiment comprises the following specific steps:
(1) Prefractionation of crude benzene:
pre-fractionating raw material of crude benzene 11, wherein the temperature of a tower kettle 3 is 170 ℃, the pressure of the tower kettle is-40 kPa, and removing low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
by increasing the temperature of the tower bottom of the pre-distillation tower, the content of 'triphenyl' (benzene, toluene and xylene) in the product after pre-distillation treatment is slightly increased, and the content of high boiling point solvent oil taking C9 components as main fractions is increased, but the mass fraction of the nitrogen-containing compounds contained in the product is increased. Mixing the prefractionated material with hydrogen, heating and pressurizing, introducing into a first hydrogenation reactor 102 and a second hydrogenation reactor 103, wherein the first hydrogenation reactor adopts a NiMo catalyst, and the filling density is 0.7g/cm for improving the hydrodenitrogenation performance of hydrofining, wherein the NiMo catalyst is CNBR-01-southwest chemical engineering institute of research, inc 3 The conventional part of CoMo catalyst was replaced with NiMo catalyst in the second hydrogenation reactor 103, wherein the mass ratio of NiMo to CoMo was 1:4 and the packing density was 0.75g/cm 3 CoMo catalyst type CNBR-02 southwest chemical engineering research institute Co., ltd, the reaction temperature and the reaction pressure remain unchanged.
(3) And (3) rectifying and separating:
and (2) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower 104 and a second rectifying tower 105, high-purity benzene and toluene are respectively extracted from the tops of the first rectifying tower 104 and the second rectifying tower 105, a side line extraction process is adopted, a side line extraction port is positioned on a 59 th column plate, the temperature of the column plate is controlled to 145 ℃, the temperature of a column bottom is 161 ℃, the pressure of the column bottom is 55kPa, and xylene 18 and high-boiling solvent oil 19 are respectively extracted from the side line and the column bottom of the second rectifying tower.
Example 4
As shown in FIG. 1, the NiMo catalyst CNBR-01-southwest chemical industry institute, co catalyst is M8-12, and the method for refining crude benzene and by-producing high-boiling solvent oil comprises the following specific steps:
(1) Prefractionation of crude benzene:
pre-fractionating raw material of crude benzene 11, wherein the temperature of a tower kettle is 170 ℃, the pressure of the tower kettle is-30 kPa, and removing low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
by increasing the temperature of the tower bottom of the pre-distillation tower, the content of 'triphenyl' (benzene, toluene and xylene) in the product after pre-distillation treatment is slightly increased, and the content of high boiling point solvent oil taking C9 components as main fractions is increased, but the mass fraction of the nitrogen-containing compounds contained in the product is increased. Mixing the prefractionated material with hydrogen, heating and pressurizing, introducing into a first hydrogenation reactor and a second hydrogenation reactor, wherein the first hydrogenation reactor adopts a NiMo catalyst, and in order to improve the hydrodenitrogenation performance of hydrofining, the second hydrogenation reactor replaces the traditional part of CoMo catalyst with NiMo catalyst, wherein the mass ratio of NiMo to CoMo is 1:3, and the packing density is 0.73g/cm 3 Reaction temperature the reaction pressure remained unchanged.
(3) And (3) rectifying and separating:
and (3) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower 104 and a second rectifying tower 105, high-purity benzene and toluene are respectively extracted from the tops of the first rectifying tower 104 and the second rectifying tower 105, a side line extraction process is adopted, a side line extraction outlet is positioned on a 55 th column plate, the temperature of the column plate is controlled to be 143 ℃, the temperature of a column bottom is controlled to be 165 ℃, the pressure of the column bottom is 60kPa, and xylene and high-boiling-point solvent oil are respectively extracted from the side line and the column bottom of the second rectifying tower 105.
Example 5
As shown in fig. 1, the method for refining crude benzene and by-producing high boiling solvent oil in this embodiment comprises the following specific steps:
(1) Prefractionation of crude benzene:
pre-fractionating the raw material of crude benzene 11, wherein the temperature of a tower kettle 3 is 165 ℃, the pressure of the tower kettle is-35 kPa, and removing low boiling point compounds and heavy benzene components;
(2) Hydrofining of crude benzene:
mixing the prefractionated material with hydrogen, heating and pressurizing, introducing into a first hydrogenation reactor 102 and a second hydrogenation reactor 103, wherein the first hydrogenation reactor 102 and the second hydrogenation reactor 103 are CoMo catalysts, the CoMo catalysts are M8-12, and the packing density is 0.7g/cm 3 Reaction temperature the reaction pressure remained unchanged.
(3) And (3) rectifying and separating:
and (3) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower 104 and a second rectifying tower 105, high-purity benzene is extracted from the top of the first rectifying tower 104, high-purity toluene is extracted from the top of the second rectifying tower 105, dimethylbenzene is extracted from the tower kettle, the side line extraction process is omitted, the temperature of the tower kettle is 165 ℃, and the pressure of the tower kettle is 60kPa.
The mass fraction results of toluene, xylene and C9 component high boiling point solvent oil in the second rectifying column of examples 1 to 5 are shown in Table 1.
TABLE 1 mass fractions of toluene, xylene and C9 component high boiling point solvent oils in the second rectification column
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (5)
1. The method for refining the byproduct high-boiling-point solvent oil from the crude benzene is characterized by comprising the following specific steps of: (1) crude benzene prefractionation: prefractionating the crude benzene raw material to remove low boiling point compounds and heavy benzene components; (2) hydrofining of crude benzene: mixing the prefractionated material with hydrogen, heating and pressurizing, introducing the mixture into a first hydrogenation reactor and a second hydrogenation reactor, respectively carrying out unsaturated component hydrogenation reaction, hydrodesulfurization and hydrodenitrogenation reaction, and removing sulfur-containing and nitrogen-containing mixtures, thereby producing high-quality aromatic compounds such as benzene, toluene and xylene; (3) rectifying and separating: and (3) after the liquid phase material obtained in the step (2) is treated by other working procedures, the liquid phase material is led into a first rectifying tower and a second rectifying tower, high-purity benzene and toluene are respectively extracted from the tops of the first rectifying tower and the second rectifying tower, a side line extraction process is adopted, and xylene and high-boiling solvent oil are respectively extracted from the side line and the tower bottom of the second rectifying tower.
2. The method for producing high boiling solvent oil as claimed in claim 1, wherein in the step (1), the temperature of the pre-distillation column bottom is 160-175 ℃ and the pressure is-30 to-40 kPa.
3. The method for producing high boiling point solvent oil as defined in claim 1, wherein in the step (2), the first hydrogenation reactor is a NiMo catalyst, the second hydrogenation reactor is filled with NiMo catalyst and CoMo catalyst, and the filling ratio of NiMo catalyst to CoMo catalyst is 1: 19-1: 3, wherein NiMo catalyst MoO 3 The content is 8-12 wt%.
4. The method for producing high boiling solvent oil as claimed in claim 1, wherein in the step (3), the temperature of the second rectifying tower is 150-165 ℃ and the pressure is 45-60 kpa.
5. The method for producing high boiling point solvent oil as claimed in claim 1, wherein in the step (3), the side offtake positions are 55 to 62 pieces, and the tray temperature is 143 to 146 ℃.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211093852 | 2022-09-08 | ||
| CN2022110938520 | 2022-09-08 |
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| CN116640603A true CN116640603A (en) | 2023-08-25 |
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| CN202211278531.8A Pending CN116640603A (en) | 2022-09-08 | 2022-10-19 | Method for refining crude benzene and preparing byproduct high-boiling-point solvent oil |
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| CN (1) | CN116640603A (en) |
| WO (1) | WO2024051737A1 (en) |
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| WO2024051737A1 (en) * | 2022-09-08 | 2024-03-14 | 淮北师范大学 | Method for producing high boiling point solvent oil byproduct in crude benzene refinement |
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| FR1186934A (en) * | 1956-04-11 | 1959-09-03 | Metallgesellschaft Ag | Process for extracting pure aromatic hydrocarbons from crude benzene |
| CN100378046C (en) * | 2006-07-06 | 2008-04-02 | 湖南长岭石化科技开发有限公司 | Method for producing benzene aromatic hydrocarbon from crude benzole |
| CN103013560A (en) * | 2011-09-26 | 2013-04-03 | 花得水 | Method for extracting solvent oil with high boiling point from crude benzol |
| CN103520945B (en) * | 2012-07-04 | 2016-05-25 | 天津大学 | The refining plant of crude benzole hydrogenation product and method |
| DE102012111292A1 (en) * | 2012-11-22 | 2014-05-22 | Thyssenkrupp Uhde Gmbh | Process for the isolation of benzene, toluene and xylene from an aromatics-rich feed gas stream |
| CN106916044A (en) * | 2015-12-24 | 2017-07-04 | 上海宝钢化工有限公司 | A kind of method for refining carbonization crude benzole |
| CN105646126B (en) * | 2016-03-07 | 2018-10-23 | 南京师范大学 | The separation method of toluene, dimethylbenzene, trimethylbenzene in a kind of aromatic solvent naphtha |
| CN116640603A (en) * | 2022-09-08 | 2023-08-25 | 临涣焦化股份有限公司 | Method for refining crude benzene and preparing byproduct high-boiling-point solvent oil |
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| WO2024051737A1 (en) * | 2022-09-08 | 2024-03-14 | 淮北师范大学 | Method for producing high boiling point solvent oil byproduct in crude benzene refinement |
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