CN107353926A - A kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene - Google Patents

A kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene Download PDF

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Publication number
CN107353926A
CN107353926A CN201710580406.5A CN201710580406A CN107353926A CN 107353926 A CN107353926 A CN 107353926A CN 201710580406 A CN201710580406 A CN 201710580406A CN 107353926 A CN107353926 A CN 107353926A
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CN
China
Prior art keywords
naphthalene
aromatic solvent
heavy aromatic
therefrom
refined
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710580406.5A
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Chinese (zh)
Inventor
顾正桂
徐荣昌
曹晓艳
孔瑞用
徐瑜
华琳
董小春
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Jiangsu Five Ocean Hydrocarbon Technology Co Ltd
Nanjing Normal University
Original Assignee
Jiangsu Five Ocean Hydrocarbon Technology Co Ltd
Nanjing Normal University
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Application filed by Jiangsu Five Ocean Hydrocarbon Technology Co Ltd, Nanjing Normal University filed Critical Jiangsu Five Ocean Hydrocarbon Technology Co Ltd
Priority to CN201710580406.5A priority Critical patent/CN107353926A/en
Publication of CN107353926A publication Critical patent/CN107353926A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G7/00Distillation of hydrocarbon oils
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/14Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1096Aromatics or polyaromatics

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A kind of the invention discloses No. 1500 heavy aromatic solvent oil lightings and therefrom method of refined naphthalene, this method remove naphthalene in No. 1500 heavy aromatic solvent oils using continuous decompression side line rectifying, and side run-off is through continuation column tubular type crystallization apparatus, therefrom refined naphthalene.Relative to prior art, present invention process is simple, can operate continuously, and naphthalene content≤2.0%, lightweight heavy aromatic solvent oil yield >=88.30% in No. 1500 lightweight heavy aromatic solvent oils after separation, refines naphthalene content >=96.20%, yield >=87.67%.

Description

A kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene
Technical field
A kind of the invention discloses No. 1500 heavy aromatic solvent oil lightings and therefrom method of refined naphthalene, belongs to heavy aromatics Solvent naphtha technical field of refinement.
Background technology
No. 1500 heavy aromatic solvent oils refer to the C of the by-product in oil and coal process9、C10、C11And C11Above aromatic hydrocarbons Solvent, the solvent has flash-point height, toxicity is low, smell is small, dissolving power is strong, evaporation rate is moderate, emulsifiability is good and performance is steady The features such as determining, be production coating resin, high-grade paint, coating, ink, adhesive, paint thinner, agricultural chemicals (emulsifying agent), The ideal solvent of aluminum paste, the ideal solvent of hydrogen peroxide and electrostatic painting, is alternatively arranged as high-temperature chemical reaction solvent and oil adds Add agent production solvent and industrial cleaning agent etc., heavy aromatic solvent oil has preferable compatibility with polyvinyl chloride resin, can be used to replacement two Butyl ester, dioctyl ester as production PVC plastic material products plasticizer, such as produce plastic flexible pipe, sealing strip, plastic shoes, artificial leather and Cable cover(ing) etc..
In No. 1500 heavy aromatic solvent oils, because naphthalene content is higher than 8%, solvent naphtha use range and use have impact on Amount.At present, it is main in industrial production that naphthalene in cut or multiple rectifying No. 1500 solvent naphthas of removing is cut using distillation, naphthalene content is dropped As little as less than 3%, then using letter have a rest crystallization or multistage crystallization method refined naphthalene.Using distillation or multiple rectification method removing naphthalene, deposit In complex disposal process, product yield is low and the big problem of energy consumption, while naphthalene ends content is low after separating, and is unfavorable for the refined of naphthalene.
The content of the invention
Goal of the invention:In order to make up the above-mentioned deficiency of existing production, the present invention provides a kind of No. 1500 heavy aromatic solvent oils The method that lighting refines with naphthalene, the method combined is crystallized with tubulation using decompression side line rectifying and removes No. 1500 aromatic solvent naphthas In naphthalene, and refined naphthalene.The process is simple, No. 1500 lightweight heavy aromatic solvent oil yields are low up to more than 88.30%, energy consumption, The content and yield of naphthalene reach 96.20% and more than 87.67%.
Technical scheme:A kind of the invention provides No. 1500 heavy aromatic solvent oil lightings and therefrom method of refined naphthalene, Naphthalene in No. 1500 heavy aromatic solvent oils is removed using continuous decompression side line rectifying, side run-off through continuation column tubular type crystallization apparatus, Therefrom refined naphthalene, specifically comprise the following steps:
(1) No. 1500 heavy aromatic solvent oils of raw material add from the middle and upper part of decompression side line rectifying column, the pressure of control tower, surely Determine tower top and bottom temperature, after being separated, it is No. 1500 lightweight heavy aromatic solvent oils that tower top, which distillates component, and side line is concentrating naphthalene Cut, bottom are triethylbenzene (TEB) cut;
(2) the concentrating naphthalene cut that side line distillates is squeezed into continuation column tubular type crystallization apparatus, and it is in parallel that the device includes several Tubulation crystallizer, by cooling medium, crystallization temperature is controlled at 21~23 DEG C, certain time is stopped, from tubulation crystallizer bottom Non- crystalline mother solution is collected in portion, and then by heating medium, control tubulation mould temperature is kept for certain time at 80~82 DEG C, From bottom collection, the naphthalene after refining is produced.
It is preferred that the pressure of control tower is 0.015Mpa in step (1), stable tower top and bottom temperature are:Tower top temperature is 128.5~130.2 DEG C, bottom temperature is 162.2~164.8 DEG C.
Naphthalene content≤2.0% in No. 1500 lightweight heavy aromatic solvent oils obtained by step (1).
It is preferred that crystallization temperature control stops 60 minutes at 21~23 DEG C in step (2);Control tubulation mould temperature exists 80~82 DEG C, kept for 60 minutes.
It is preferred that the quantity of tubulation crystallizer described in step (2) is 2, transcrystallization, feed time are carried out during its work It is separated by 60 minutes.
Naphthalene after gained is refined in step (2), wherein naphthalene content reach more than 96.20%.
In the inventive method, decompression side line rectifying column is using conventional decompression side line rectifying column.
In the above method, naphthalene content is 10% or so in raw material, and decompression side line inlet amount is 10Kg/h, other concrete technologies Parameter is preferably as follows shown in table 1:
Table 1 depressurizes side line rectifying and tubulation 4 Crystallization
Technique effect:Relative to prior art, the inventive method technique is simple, can operate continuously, No. 1500 light after separation Naphthalene content≤2.0%, yield >=88.30% in matter heavy aromatic solvent oil, naphthalene content >=96.20%, yield after crystallization >= 87.67%.
Brief description of the drawings
Fig. 1 is the technological process and equipment connecting relation figure of the inventive method:Including decompression side line rectifying column 1, condenser 2nd, side line discharge 3, reboiler 4, intermediate storage tank 5, visor 6, tubulation crystallizer 7, tubulation crystallizer 8, material feed pump 9, plus Thermal medium charging aperture 10, heating pipe outlet 11, coolant feed pipe inlet 12, cooling medium discharging opening 13, k1~k16 valves Door.
Embodiment
Below in conjunction with the accompanying drawings and instantiation, the present invention is furture elucidated, it should be understood that these examples are merely to illustrate this hair Bright rather than limitation the scope of the present invention.
Embodiment 1
The technique that a kind of No. 1500 heavy aromatic solvent oil lightings refine with naphthalene, as shown in Figure 1:
(1) 1. raw material adds from the 25th piece of position of decompression side line rectifying column 1, and the pressure of control tower is 0.015MPa, when Tower top, bottom temperature start stabilization, and tower top temperature is 128.5~130.2 DEG C, and bottom temperature is 162.2~164.8 DEG C, after separation, 2. overhead components are No. 1500 lightweight heavy aromatic solvent oils, naphthalene content≤2.0%, 3. side line is the component of 51.85% naphthalene of enrichment, 4. bottom is triethylbenzene (TEB) cut;
(2) side line distillates concentrating naphthalene cut and 3. enters intermediate storage tank 5, and continuation column tubular type crystallization apparatus 7 is squeezed into by pump 9 In, k5 and k7 cooling medium valves are opened, at 21~23 DEG C, the residence time is 60 minutes, opens tubulation knot for crystallization temperature control Brilliant device bottom valve k15, collect non-crystalline mother solution 6., be then shut off k5, k7 and k15, open k9, k11, by heating medium, The temperature control of tubulation crystallizer 7 is controlled to open k13 at 80~82 DEG C, 60 minutes, collection obtains 5. more than 96.20% naphthalene, yield Reach 87.67%;
(3) tubulation crystallizer 8 is equally operated according to tubulation crystallizer 7, and tubulation crystallizer 7 and tubulation crystallizer 8 enter Row transcrystallization, feed time are separated by 60 minutes.Whole process process conditions are as shown in table 2, as a result as shown in table 3.
The side line rectifying of table 2 combines removing naphthalene and naphthalene process for refining condition with tubulation crystallization
The side line rectifying of table 3 combines removing naphthalene and naphthalene upgrading result with tubulation crystallization

Claims (6)

1. a kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene, it is characterised in that using continuous decompression Side line rectifying removes naphthalene in No. 1500 heavy aromatic solvent oils, and side run-off is through continuation column tubular type crystallization apparatus, and therefrom refined naphthalene, has Body comprises the following steps:
(1) No. 1500 heavy aromatic solvent oils of raw material add from the middle and upper part of decompression side line rectifying column, the pressure of control tower, stabilizer Top and bottom temperature, after being separated, it is No. 1500 lightweight heavy aromatic solvent oils that tower top, which distillates component, and side line evaporates for concentrating naphthalene Point, bottom is triethylbenzene (TEB) cut;
(2) the concentrating naphthalene cut that side line distillates is squeezed into continuation column tubular type crystallization apparatus, and the device includes several row in parallel Pipe crystallizer, by cooling medium, crystallization temperature is controlled at 21~23 DEG C, stops certain time, is received from tubulation crystalliser feet The non-crystalline mother solution of collection, then by heating medium, control tubulation mould temperature is kept for certain time, the bottom of from 80~82 DEG C Portion is collected, and produces the naphthalene after refining.
2. No. 1500 heavy aromatic solvent oil lightings according to claim 1 and therefrom the method for refined naphthalene, its feature exist In the pressure of control tower is 0.015Mpa in step (1), and stable tower top and bottom temperature are:Tower top temperature is 128.5~130.2 DEG C, bottom temperature is 162.2~164.8 DEG C.
3. No. 1500 heavy aromatic solvent oil lightings according to claim 1 and therefrom the method for refined naphthalene, its feature exist In naphthalene content≤2.0% in No. 1500 lightweight heavy aromatic solvent oils obtained by step (1).
4. No. 1500 heavy aromatic solvent oil lightings according to claim 1 and therefrom the method for refined naphthalene, its feature exist In crystallization temperature control is at 21~23 DEG C in step (2), stop 60 minutes;Tubulation mould temperature is controlled to be protected at 80~82 DEG C Hold 60 minutes.
5. No. 1500 heavy aromatic solvent oil lightings according to claim 1 and therefrom the method for refined naphthalene, its feature exist It is 2 in, the quantity of tubulation crystallizer described in step (2), carries out transcrystallization during its work, feed time is separated by 60 points Clock.
6. No. 1500 heavy aromatic solvent oil lightings according to claim 1 and therefrom the method for refined naphthalene, its feature exist In the naphthalene after gained is refined in step (2), wherein naphthalene content reaches more than 96.20%.
CN201710580406.5A 2017-07-17 2017-07-17 A kind of No. 1500 heavy aromatic solvent oil lightings and the therefrom method of refined naphthalene Pending CN107353926A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115746905A (en) * 2022-11-24 2023-03-07 鹏辰新材料科技股份有限公司 Production method of special solvent oil for hydrogen peroxide

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474492A (en) * 2008-12-23 2009-07-08 南京师范大学 Method and equipment for preparing super fine powder using ceramic film antisolvent coupling process in semi-continuous type
CN104496907A (en) * 2015-01-07 2015-04-08 江苏沿江化工资源开发研究院有限公司 Method for refining imidazole through combination of continuous reduced-pressure side stream rectification and roller crystallization
CN104892347A (en) * 2015-06-24 2015-09-09 南京师范大学 Method for using continuous lateral line distillation and continuous crystallization integration to extract methylnaphthalene in C10 aromatics
CN105272815A (en) * 2014-06-10 2016-01-27 中国石化扬子石油化工有限公司 Method for extracting methylnaphthalene in C10 aromatics

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474492A (en) * 2008-12-23 2009-07-08 南京师范大学 Method and equipment for preparing super fine powder using ceramic film antisolvent coupling process in semi-continuous type
CN105272815A (en) * 2014-06-10 2016-01-27 中国石化扬子石油化工有限公司 Method for extracting methylnaphthalene in C10 aromatics
CN104496907A (en) * 2015-01-07 2015-04-08 江苏沿江化工资源开发研究院有限公司 Method for refining imidazole through combination of continuous reduced-pressure side stream rectification and roller crystallization
CN104892347A (en) * 2015-06-24 2015-09-09 南京师范大学 Method for using continuous lateral line distillation and continuous crystallization integration to extract methylnaphthalene in C10 aromatics

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
周永兵: "连续侧线出料精馏法和连续结晶法提取C10芳烃中均四甲苯馏分", 《万方数据库》 *
顾正桂: "《化工分离单元集成技术及应用》", 30 April 2010, 化学工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115746905A (en) * 2022-11-24 2023-03-07 鹏辰新材料科技股份有限公司 Production method of special solvent oil for hydrogen peroxide

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