CN109181760B - Production method of aromatic oil - Google Patents
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- CN109181760B CN109181760B CN201811276216.5A CN201811276216A CN109181760B CN 109181760 B CN109181760 B CN 109181760B CN 201811276216 A CN201811276216 A CN 201811276216A CN 109181760 B CN109181760 B CN 109181760B
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- raffinate
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- 239000010692 aromatic oil Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 52
- 239000003921 oil Substances 0.000 claims abstract description 29
- 239000003463 adsorbent Substances 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 17
- 238000001179 sorption measurement Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 19
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 16
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 8
- 241001122767 Theaceae Species 0.000 claims description 7
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 7
- 235000013824 polyphenols Nutrition 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 239000010721 machine oil Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000010074 rubber mixing Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000008096 xylene Substances 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
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for producing aromatic oil, and relates to the technical field of petrochemical industry. The invention adopts the multistage extraction tower to replace the existing packed tower as the extraction tower, thereby obviously improving the production efficiency; after extraction is finished, removing water and inorganic impurities in raffinate oil and non-aromatic organic impurities by adopting an adsorbent adsorption separation method, so that the purity of aromatic oil is improved; meanwhile, due to the removal of impurities, the viscosity of the aromatic oil is uniform, and the use efficiency of the aromatic oil is improved.
Description
The technical field is as follows:
the invention relates to the technical field of petrochemical industry, in particular to a method for producing aromatic oil.
Background art:
aromatic oil is one of basic raw materials of petrochemical industry, and mainly comprises benzene, toluene and xylene. It can soften and plasticize rubber. Finally, the effect of changing the elasticity and the toughness of the rubber is achieved. It is mainly used in the rubber mixing process of rubber and tyre. Under the condition of high temp. and high pressure, petroleum is gradually decomposed into gasoline, machine oil, wax oil and residual oil. The aromatic oil is a product obtained after the residual oil is subjected to a series of reactions of catalysis and cracking.
At present, aromatic oil generally has the problems of too much water, uneven viscosity and less aromatic hydrocarbon content, which brings many adverse factors to production and application.
In addition, in the process of producing the environment-friendly aromatic oil, an extraction tower is usually required, the conventional extraction tower basically adopts a traditional filler extraction tower, and the filler extraction tower is difficult to ensure the sufficient contact of a solvent and materials due to the high viscosity of the materials, so that the extraction efficiency of the tower is low, and the ideal extraction effect cannot be achieved.
The invention content is as follows:
the invention aims to solve the technical problem of providing a method for producing aromatic oil with low moisture content, uniform viscosity and high aromatic hydrocarbon content.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for producing aromatic oil, comprising the steps of:
(1) extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the temperature at the top of the extraction tower is 60-80 ℃, and an effluent liquid is a raffinate; the temperature of the bottom of the extraction tower is 45-70 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 30-80 r/min, the solvent-oil ratio is 0.5-2: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 100-160 ℃.
The multistage extraction tower can disperse materials into more uniform and reasonable liquid drops, so that the continuous phase and the dispersed phase are fully contacted, the aim of simultaneously completing a plurality of extraction processes is fulfilled, and the multistage extraction tower has high extraction efficiency.
The preparation method of the adsorbent comprises the following steps:
(1) soaking montmorillonite in deionized water for 10-30min to remove surface impurities, drying in a drying oven to constant weight, pulverizing, and sieving with 100-fold 150-mesh sieve;
(2) adding the sieved montmorillonite into 25-40 wt% acetic acid solution, stirring at 70-80 deg.C for 10-30min, adding tea polyphenols, and stirring for 30-50 min;
(3) and (3) adding a titanate coupling agent and dicumyl peroxide into the mixed solution obtained in the step (2), heating to a reflux state, keeping the temperature and stirring for 0.5-2h, filtering while hot, washing the solid with deionized water and absolute ethyl alcohol to remove impurities, and drying in vacuum at 50 ℃ to constant weight to obtain the adsorbent.
The mass ratio of the montmorillonite to the acetic acid solution to the tea polyphenol to the titanate coupling agent to the dicumyl peroxide is 20-40: 80-200: 3-5: 5-10: 0.1-0.2.
Adsorption principle of the adsorbent: during acid treatment, acetic acid exchanges calcium ions and sodium ions in the montmorillonite to form pore channels, so that a plurality of pores are generated, meanwhile, hydrogen ions can dissolve part of inorganic ions in the aluminum octahedron, the bonding force between layers is weakened, and the adsorbability of the montmorillonite on inorganic substances such as water molecules is improved; meanwhile, the titanate coupling agent is coupled between molecules under the action of dicumyl peroxide and is bonded in the montmorillonite, so that the adsorbability of the montmorillonite on organic impurities is improved.
The invention has the beneficial effects that: the invention adopts the multistage extraction tower to replace the existing packed tower as the extraction tower, thereby obviously improving the production efficiency; after extraction is finished, removing water and inorganic impurities in raffinate oil and non-aromatic organic impurities by adopting an adsorbent adsorption separation method, so that the purity of aromatic oil is improved; meanwhile, due to the removal of impurities, the viscosity of the aromatic oil is uniform, and the use efficiency of the aromatic oil is improved.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the tower top temperature of the extraction tower is 60 ℃, and effluent liquid is raffinate; the temperature of the bottom of the extraction tower is 50 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 40 r/min, the solvent-oil ratio is 0.5: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 120 ℃;
preparation of the adsorbent:
(1) soaking 20kg of montmorillonite in deionized water for 20min to remove surface impurities, drying in a drying oven to constant weight, pulverizing, and sieving with a 150-mesh sieve of 100 meshes;
(2) adding the sieved montmorillonite into 100kg of 30% acetic acid solution, stirring at 70 deg.C for 30min, adding 3kg of tea polyphenols, and stirring for 50 min;
(3) and (3) adding 5kg of titanate coupling agent and 0.1kg of dicumyl peroxide into the mixed solution in the step (2), heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing the solid with deionized water and absolute ethyl alcohol to remove impurities, and drying in vacuum at 50 ℃ to constant weight to obtain the adsorbent.
Example 2
(1) Extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the temperature at the top of the extraction tower is 80 ℃, and effluent liquid is raffinate; the temperature of the bottom of the extraction tower is 60 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 50 revolutions per minute, the agent-oil ratio is 0.8: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 140 ℃;
preparation of the adsorbent:
(1) soaking 20kg of montmorillonite in deionized water for 20min to remove surface impurities, drying in a drying oven to constant weight, pulverizing, and sieving with a 150-mesh sieve of 100 meshes;
(2) adding the sieved montmorillonite into 100kg of 30% acetic acid solution, stirring at 70 deg.C for 30min, adding 3kg of tea polyphenols, and stirring for 50 min;
(3) and (3) adding 5kg of titanate coupling agent and 0.1kg of dicumyl peroxide into the mixed solution in the step (2), heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing the solid with deionized water and absolute ethyl alcohol to remove impurities, and drying in vacuum at 50 ℃ to constant weight to obtain the adsorbent.
Comparative example 1
(1) Extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the tower top temperature of the extraction tower is 60 ℃, and effluent liquid is raffinate; the temperature of the bottom of the extraction tower is 50 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 40 r/min, the solvent-oil ratio is 0.5: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 120 ℃;
preparation of the adsorbent:
(1) soaking 20kg of montmorillonite in deionized water for 20min to remove surface impurities, drying in a drying oven to constant weight, pulverizing, and sieving with a 150-mesh sieve of 100 meshes;
(2) adding the sieved montmorillonite into 100kg of acetic acid solution with the mass fraction of 30%, stirring for 30min at 70 ℃, and then continuing to stir for 50 min;
(3) and (3) adding 5kg of titanate coupling agent and 0.1kg of dicumyl peroxide into the mixed solution in the step (2), heating to a reflux state, keeping the temperature and stirring for 2h, filtering while hot, washing the solid with deionized water and absolute ethyl alcohol to remove impurities, and drying in vacuum at 50 ℃ to constant weight to obtain the adsorbent.
Comparative example 2
(1) Extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the tower top temperature of the extraction tower is 60 ℃, and effluent liquid is raffinate; the temperature of the bottom of the extraction tower is 50 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 40 r/min, the solvent-oil ratio is 0.5: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 120 ℃;
adsorbent: activated carbon FX-40 adsorbent.
Example 3
Based on example 1, comparative example 1 in which tea polyphenol was not added and comparative example 2 in which activated carbon FX-40 was used as an adsorbent were provided.
Aromatic oils were prepared according to examples 1-2 and comparative examples 1-2, and the properties of the aromatic oils were measured, and the results are shown in Table 1.
TABLE 1 Performance testing of aromatic oils
| Test items | Kinematic viscosity (37 ℃ C.) | Moisture content (%) | CA(％) |
| Example 1 | 489.61 | ≤0.01 | 38 |
| Example 2 | 490.32 | ≤0.01 | 37 |
| Comparative example 1 | 485.47 | 0.019 | 33 |
| Comparative example 2 | 482.85 | 0.023 | 29 |
Kinematic viscosity: ASTM D445; moisture content: ASTM D95;
CA refers to the percentage of aromatic carbon number in the average molecular structure to the total carbon number, and the test method is ASTM D2140.
The experimental data show that the quality of the aromatic oil prepared by the production method is completely qualified, and the production method of the aromatic oil is worthy of popularization and can realize industrial production.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. A method for producing aromatic oil is characterized by comprising the following steps:
(1) extracting aromatic oil in an extraction tower by taking aromatic oil as a raw material and furfural as a solvent, wherein the temperature at the top of the extraction tower is 60-80 ℃, and an effluent liquid is a raffinate; the temperature of the bottom of the extraction tower is 45-70 ℃, and the effluent liquid is an extract liquid; the rotating speed of the extraction tower is 30-80 r/min, and the agent-oil ratio is 0.5-2: 1; the extraction tower is a multi-stage extraction tower;
(2) heating raffinate obtained in the step 1 by using heat transfer oil under negative pressure to remove furfural to obtain raffinate oil, and feeding the raffinate oil into an adsorption tower containing an adsorbent to adsorb to obtain purified aromatic oil; the bed temperature of the adsorption tower is 100-160 ℃;
the preparation method of the adsorbent comprises the following steps:
(1) soaking montmorillonite in deionized water for 10-30min to remove surface impurities, drying in a drying oven to constant weight, pulverizing, and sieving with 100-fold 150-mesh sieve;
(2) adding the sieved montmorillonite into 25-40 wt% acetic acid solution, stirring at 70-80 deg.C for 10-30min, adding tea polyphenols, and stirring for 30-50 min;
(3) and (3) adding a titanate coupling agent and dicumyl peroxide into the mixed solution obtained in the step (2), heating to a reflux state, keeping the temperature and stirring for 0.5-2h, filtering while hot, washing the solid with deionized water and absolute ethyl alcohol to remove impurities, and drying in vacuum at 50 ℃ to constant weight to obtain the adsorbent.
2. The method for producing an aromatic oil according to claim 1, characterized in that: the mass ratio of the montmorillonite to the acetic acid solution to the tea polyphenol to the titanate coupling agent to the dicumyl peroxide is 20-40: 80-200: 3-5: 5-10: 0.1-0.2.
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| CN201811276216.5A CN109181760B (en) | 2018-10-30 | 2018-10-30 | Production method of aromatic oil |
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| CN201811276216.5A CN109181760B (en) | 2018-10-30 | 2018-10-30 | Production method of aromatic oil |
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| CN109181760B true CN109181760B (en) | 2021-04-13 |
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Effective date of registration: 20240204 Address after: 243000 No.1 Chaosan Road, Provincial Fine Chemical Base, Hexian Economic Development Zone, Ma'anshan City, Anhui Province Patentee after: Anhui Jubaoshi Technology Co.,Ltd. Country or region after: China Address before: 238200 Fine Chemical Base of Wujiang Town, Ma'anshan City and County, Anhui Province Patentee before: ANHUI HAIDE CHEMICAL TECHNOLOGY Co.,Ltd. Country or region before: China |