CN103288584A - Process method for extracting high-purity beta-methylnaphthalene from reformed aromatic hydrocarbon C10 - Google Patents
Process method for extracting high-purity beta-methylnaphthalene from reformed aromatic hydrocarbon C10 Download PDFInfo
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Abstract
The invention relates to a process method for extracting high-purity beta-methylnaphthalene from reformed aromatic hydrocarbon C10. The process method comprises the following steps of: by taking catalytically reformed by-product hydrocarbon C10 as a raw material and refined components as raw materials after carrying out rectification, freezing crystallization and refining on the catalytically reformed by-product hydrocarbon C10, putting the raw materials into a multistage countercurrent fractional crystallizer, and refining and extracting the beta-methylnaphthalene, so as to obtain the beta-methylnaphthalene with the purity high than 99%. The process method has the advantages of simple process, relatively low equipment investment and production cost, no polluted by-product and relatively high economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of reformation aromatic hydrocarbons C
10The middle processing method of extracting high-purity beta-methylnaphthalene is with catalytic reforming by product aromatic hydrocarbons C
10Be raw material, through the processing method of rectifying, freezing and crystallizing, refining back extraction high-purity beta-methylnaphthalene.
Background technology
Beta-methylnaphthalene is a kind of white crystals with similar naphthalene smell, mainly for the production of vitamin K
3, can also have a wide range of applications in field of fine chemical as the raw material of fine chemical products such as sterilant, medicine intermediate, dyestuff.
Beta-methylnaphthalene extracts from the coal tar wash oil cut usually, but because coal tar complicated component, contain acidity and alkaline matter, need to extract through acid-alkali washing, whole extraction process process complexity is loaded down with trivial details, is unfavorable for reducing cost, and produced simultaneously by product pollutes environment, therefore, from other raw materials, extract the focus that beta-methylnaphthalene becomes Recent study.Catalytic reforming by product aromatic hydrocarbons C
10Middle beta-methylnaphthalene content is higher, and composition is more single, is the desirable feedstock of extracting beta-methylnaphthalene; Simultaneously, domestic manufacturer's beta-methylnaphthalene product purity is lower, 95
-Between 97%, and high-end field such as pharmaceutical industries need product purity more than 99%, can not satisfy the demand of high-end field.The technology of general rectifying and freezing and crystallizing is expected purity at the beta-methylnaphthalene more than 99%, and yield is extremely low, and cost is too high, can not meet the need of market; And adopt entrainer (as ethylene glycol) by azeotropic distillation, though can obtain the beta-methylnaphthalene product of purity more than 99%, owing to use entrainer, cost is also higher.
Opening The First has led (by C
10Heavy aromatics separates preparation high-purity beta-methylnaphthalene, Speciality Petrochemicals, in May, 1996, the 3rd phase) with by-product C
10Heavy aromatics is raw material, prepares the methylnaphthalene (containing β-methylnaphthalene and alpha-methyl-naphthalene) of purity 〉=90% by rectifying separation, through freezing, separate that to make purity be 97% beta-methylnaphthalene.With ethyl alcohol recrystallization or can make the beta-methylnaphthalene of high purity (99%) with the solvent wash method.This method complex process is used a large amount of solvents, and cost is higher, and productive rate is lower.
Summary of the invention
The purpose of this invention is to provide a kind of new reformation aromatic hydrocarbons C
10The middle processing method of extracting high-purity beta-methylnaphthalene is with catalytic reforming by product aromatic hydrocarbons C
10Be raw material, through rectifying, freezing and crystallizing, refining back extraction beta-methylnaphthalene, can obtain the product of purity more than 99%.Technology of the present invention is simple, and facility investment is less, and production cost is lower, and pollution-free by product has high economic benefit and social benefit.
A kind of reformation aromatic hydrocarbons C provided by the invention
10The middle processing method of extracting high-purity beta-methylnaphthalene comprises:
A, rectifying are with catalytic reforming by product aromatic hydrocarbons C
10Be raw material, go out methylnaphthalene through rectifying separation, the methylnaphthalene boiling range is 235
-255 ℃, beta-methylnaphthalene content is greater than 50wt%, α
-Methylnaphthalene content is less than 30 wt%, and naphthalene content is less than 0.25wt%;
B, freezing and crystallizing are raw material with isolated methylnaphthalene, and freezing and crystallizing obtains refining component, and freezing temp is-10
-Between 10 ℃, beta-methylnaphthalene content is greater than 80wt%;
C, refining is raw material with refining component, enters the continuous multi-stage countercurrent step crystallizer and makes with extra care, and Tc is 15
-Between 35 ℃, obtain beta-methylnaphthalene content greater than the product of 99wt%;
Described reformation aromatic hydrocarbons C
10In contain 11.1927wt% durol, 10.2536 wt% naphthalenes, 13.3412 wt% beta-methylnaphthalenes, 7.4128wt% α
-The blending ingredients of methylnaphthalene and 57.7997 other components of wt%.
Described rectifying device is ripple silk net high efficiency packing rectifying tower, and rectifying adopts vacuum operating, and vacuum tightness is 0.095Mpa; Obtaining described methylnaphthalene boiling range is 235
-250 ℃, beta-methylnaphthalene content is greater than 50wt%, α
-Methylnaphthalene content is less than 30 wt%, and naphthalene content is less than 0.25wt%.
Described freezing and crystallizing equipment is inner coil pipe freezing kettle and whizzer, and freezing temp is-20
-Between 10 ℃ (preferred-10
-10 ℃), centrifugation obtains crystallization, and beta-methylnaphthalene content is greater than 80wt%;
Described purification apparatus is the continuous multi-stage countercurrent step crystallizer, and Tc is 15
-Between 35 ℃, beta-methylnaphthalene content is greater than 99wt%.
Compared with prior art, advantage of the present invention is the aromatic hydrocarbons C that reforms
10Be raw material, extract high-purity beta-methylnaphthalene, adopt rectifying, freezing and crystallizing, refining technique to carry out, can obtain the beta-methylnaphthalene of purity more than 99%.Prior art adopts the technology of rectifying and freezing and crystallizing, expect purity at the beta-methylnaphthalene more than 99%, and yield is extremely low, and cost is too high; And adopt entrainer (as ethylene glycol) by azeotropic distillation, can obtain the beta-methylnaphthalene product of purity more than 99%, but owing to use the entrainer cost higher, lack the market competitiveness.Utilize explained hereafter beta-methylnaphthalene of the present invention, cost is low, and the product purity height has high economic benefit and social benefit.
Description of drawings
Fig. 1: process flow diagram of the present invention.
Fig. 2: continuous multi-stage countercurrent step crystallizer crystallization whole process synoptic diagram.
Fig. 3: general flow chart in the crystallizer.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Wherein the beta-methylnaphthalene yield is calculated as follows:
Yield=extraction obtains beta-methylnaphthalene weighs/reformation aromatic hydrocarbons C
10The content of middle beta-methylnaphthalene.
Beta-methylnaphthalene Determination on content method: vapor-phase chromatography.
α
-The testing method of methylnaphthalene and naphthalene content: vapor-phase chromatography.
Reformation aromatic hydrocarbons C
10The source: Tianjin Petrochemical Company, form: 11.1927wt% durol, 10.2536 wt% naphthalenes, 13.3412 wt% beta-methylnaphthalenes, 7.4128wt% α
-Methylnaphthalene and other component of 57.7997 wt%.
Embodiment 1
With reformation aromatic hydrocarbons C
10Raw material 50t feeds in ripple silk net high efficiency packing (model C Y-700Y) rectifying tower continuously, and control vacuum tightness is at 0.095Mpa, and cat head obtains methylnaphthalene, boiling range 235
-254 ℃, beta-methylnaphthalene content 53.4156wt%, α
-Methylnaphthalene content 26.1324wt%, naphthalene content 0.2328wt% feeds freezing and crystallizing in the freezing kettle with methylnaphthalene, and freezing temp is-10
-Between 5 ℃, obtain refining component by the whizzer separation, beta-methylnaphthalene content 82.2567wt%, refining component feeds in the continuous multi-stage countercurrent step crystallizer, and Tc is 20
-Between 35 ℃, through the refining beta-methylnaphthalene finished product 1.52t, beta-methylnaphthalene content 99.2461wt%, beta-methylnaphthalene yield 22.79% of obtaining.
Wherein: refining component feeds in the continuous multi-stage countercurrent step crystallizer, continuous multi-stage countercurrent fractional crystallization whole process is used 3 crystallizers (following examples together) altogether, be divided into 2 step crystallizations, beta-methylnaphthalene content added No. 1 greater than 80% raw material (present embodiment beta-methylnaphthalene content 82.2567wt%) and No. 2 crystallizers in, 2 ℃/the h of speed of cooling and heating, be cooled to 28 ℃ earlier, the crystallized stock discharge is not returned the adding methylnaphthalene and is removed freezing and crystallizing, be warmed up to 36 ℃ then, the material of fusing is sent in No. 3 crystallizers, 1 ℃/the h of speed of No. 3 crystallizer coolings and heating, be cooled to 30.5 ℃ earlier, will be crystallized stock discharge return No. 1 and No. 2 crystallizers as refining raw materials, be warmed up to 36 ℃ then, with the material that melts as the qualified product extraction.(crystallizer is that Wuxi City coke gas equipment company limited produces, wherein: crystallizer tank V=20m
3).
Embodiment 2
With reformation aromatic hydrocarbons C
10Raw material 50t feeds in ripple silk net high efficiency packing (model C Y-700Y) rectifying tower continuously, and control vacuum tightness is at 0.095Mpa, and cat head obtains methylnaphthalene, boiling range 237
-255 ℃, beta-methylnaphthalene content 55.0937wt%, α
-Methylnaphthalene content 25.7332wt%, naphthalene content 0.1841wt% feeds freezing and crystallizing in the freezing kettle with methylnaphthalene, and freezing temp is-8
-Between 10 ℃, obtain refining component by the whizzer separation, beta-methylnaphthalene content 83.4622wt%, refining component feeds in the continuous multi-stage countercurrent step crystallizer, and Tc is 23
-Between 33 ℃, through the refining beta-methylnaphthalene finished product 1.61t, beta-methylnaphthalene content 99.073wt%, beta-methylnaphthalene yield 24.14% of obtaining.
Embodiment 3
With reformation aromatic hydrocarbons C
10Raw material 50t feeds in ripple silk net high efficiency packing (model C Y-700Y) rectifying tower continuously, and control vacuum tightness is at 0.095Mpa, and cat head obtains methylnaphthalene, boiling range 236
-253 ℃, beta-methylnaphthalene content 54.232wt%, α
-Methylnaphthalene content 27.5347wt%, naphthalene content 0.1966wt% feeds freezing and crystallizing in the freezing kettle with methylnaphthalene, and freezing temp is-6
-Between 10 ℃, obtain refining component by the whizzer separation, beta-methylnaphthalene content 83.2531wt%, refining component feeds in the continuous multi-stage countercurrent step crystallizer, and Tc is 22
-Between 34 ℃, through the refining beta-methylnaphthalene finished product 1.58t, beta-methylnaphthalene content 99.1463wt%, beta-methylnaphthalene yield 23.69% of obtaining.
Embodiment 4
With reformation aromatic hydrocarbons C
10Raw material 50t feeds in ripple silk net high efficiency packing (model C Y-700Y) rectifying tower continuously, and control vacuum tightness is at 0.095Mpa, and cat head obtains methylnaphthalene, boiling range 236
-254 ℃, beta-methylnaphthalene content 54.4681wt%, α
-Methylnaphthalene content 26.6212wt%, naphthalene content 0.188wt% feeds freezing and crystallizing in the freezing kettle with methylnaphthalene, and freezing temp is-10
-Between 35 ℃, obtain beta-methylnaphthalene finished product 0.93t, beta-methylnaphthalene content 99.0477wt%, beta-methylnaphthalene yield 13.94% by the whizzer separation.
Embodiment 5
With reformation aromatic hydrocarbons C
10Raw material 50t feeds in ripple silk net high efficiency packing (model C Y-700Y) rectifying tower continuously, and control vacuum tightness is at 0.095Mpa, and cat head obtains methylnaphthalene, boiling range 237
-253 ℃, beta-methylnaphthalene content 56.3879wt%, α
-Methylnaphthalene content 25.7332wt%, naphthalene content 0.1565wt% feeds freezing and crystallizing in the freezing kettle with methylnaphthalene, and freezing temp is-10
-Between 35 ℃, obtain beta-methylnaphthalene finished product 0.97t, beta-methylnaphthalene content 99.073wt%, beta-methylnaphthalene yield 14.54% by the whizzer separation.
Claims (7)
1. reformation aromatic hydrocarbons C
10The middle processing method of extracting high-purity beta-methylnaphthalene is with catalytic reforming by product aromatic hydrocarbons C
10Be raw material, through rectifying, freezing and crystallizing step, obtain refining component beta-methylnaphthalene content greater than 80wt%, it is characterized in that also comprising the steps: that with refining component be raw material, enter the continuous multi-stage countercurrent step crystallizer and make with extra care, Tc is 15
-Between 35 ℃, obtain beta-methylnaphthalene content greater than the product of 99wt%.
2. method according to claim 1 is characterized in that described with catalytic reforming by product aromatic hydrocarbons C
10Be raw material, go out methylnaphthalene through rectifying separation, the methylnaphthalene boiling range is 235
-255 ℃, beta-methylnaphthalene content is greater than 50wt%, α
-Methylnaphthalene content is less than 30 wt%, and naphthalene content is less than 0.25wt%.
3. method according to claim 1 is characterized in that described freezing and crystallizing equipment is inner coil pipe freezing kettle and whizzer, and freezing temp is-20
-Between 10 ℃, preferred freezing and crystallizing temperature is-10
-Between 10 ℃.
4. method according to claim 1 is characterized in that described reformation aromatic hydrocarbons C
10Form: 11.1927wt% durol, 10.2536 wt% naphthalenes, 13.3412 wt% beta-methylnaphthalenes, 7.4128wt% α
-Methylnaphthalene and other component of 57.7997 wt%.
5. method according to claim 1 is characterized in that Tc in the described continuous multi-stage countercurrent step crystallizer is 15
-Between 35 ℃, preferred Tc is between 23-33 ℃.
6. method according to claim 1 is characterized in that described rectifying device is ripple silk net high efficiency packing rectifying tower, and the vacuum tightness in the rectification step in the control rectifying tower is 0.092-0.098Mpa.
7. method according to claim 1, it is characterized in that continuous multi-stage countercurrent fractional crystallization whole process uses 3 crystallizers altogether, be divided into two-step crystallization, beta-methylnaphthalene content added No. 1 greater than 80% raw material and No. 2 crystallizers in, 2 ℃/the h of speed of cooling and heating, be cooled to 28 ℃ earlier, the crystallized stock discharge is not returned the adding methylnaphthalene and is removed freezing and crystallizing, be warmed up to 36 ℃ then, the material of fusing is sent in No. 3 crystallizers, 1 ℃/the h of speed of No. 3 crystallizer coolings and heating, be cooled to 30.5 ℃ earlier, will be crystallized stock discharge return No. 1 and No. 2 crystallizers as refining raw materials, be warmed up to 36 ℃ then, with the material that melts as the qualified product extraction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107652156A (en) * | 2017-11-18 | 2018-02-02 | 辽宁科技学院 | A kind of method for crystallising and device of β methyl naphthalenes |
| CN108440233A (en) * | 2018-04-17 | 2018-08-24 | 鹏辰新材料科技股份有限公司 | A method of continuously extracting beta-methylnaphthalene crude product from methyl naphthalene pregnant solution |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5798221A (en) * | 1980-12-10 | 1982-06-18 | Nippon Steel Chem Co Ltd | Production of diphenyl |
| CN101293808A (en) * | 2008-06-18 | 2008-10-29 | 华东理工大学 | Separation purification process for 2-methylnaphthalene |
-
2013
- 2013-05-13 CN CN201310173662.4A patent/CN103288584B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5798221A (en) * | 1980-12-10 | 1982-06-18 | Nippon Steel Chem Co Ltd | Production of diphenyl |
| CN101293808A (en) * | 2008-06-18 | 2008-10-29 | 华东理工大学 | Separation purification process for 2-methylnaphthalene |
Non-Patent Citations (2)
| Title |
|---|
| 孙绪峰等: "粗萘连续多级逆流分步结晶过程的研究", 《北京化工大学学报(自然科学版)》 * |
| 张竞: "由C10重芳烃分离制备高纯度β-甲基萘", 《精细石油化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107652156A (en) * | 2017-11-18 | 2018-02-02 | 辽宁科技学院 | A kind of method for crystallising and device of β methyl naphthalenes |
| CN107652156B (en) * | 2017-11-18 | 2023-11-10 | 辽宁科技学院 | Crystallization method and device of beta-methylnaphthalene |
| CN108440233A (en) * | 2018-04-17 | 2018-08-24 | 鹏辰新材料科技股份有限公司 | A method of continuously extracting beta-methylnaphthalene crude product from methyl naphthalene pregnant solution |
| CN108440233B (en) * | 2018-04-17 | 2021-02-05 | 鹏辰新材料科技股份有限公司 | Method for continuously extracting beta-methylnaphthalene crude product from methylnaphthalene enrichment solution |
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