CN1045430C - Technique for refining methyl t-butyl ether - Google Patents
Technique for refining methyl t-butyl ether Download PDFInfo
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- CN1045430C CN1045430C CN95113371A CN95113371A CN1045430C CN 1045430 C CN1045430 C CN 1045430C CN 95113371 A CN95113371 A CN 95113371A CN 95113371 A CN95113371 A CN 95113371A CN 1045430 C CN1045430 C CN 1045430C
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- butyl ether
- mtbe
- tertiary butyl
- methyl tertiary
- tower
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Abstract
The present invention relates to a technique for refining methyl tert-butyl ether. Coarse methyl tert-butyl ether with most of C4 and methanol removed through an azeotropic distillation tower is divided into light components and heavy components in the form of a liquid-phase side stream distillate in the same distillation tower to obtain refined pure methyl tert-butyl ether. The technique has the characteristics of low energy consumption, less investment, etc. The technique can be used for refining the finished product of coarse methyl tert-butyl ether.
Description
The present invention relates to the refining of methyl tertiary butyl ether, particularly, removed the process for purification of the thick methyl tertiary butyl ether of most of carbon four and methyl alcohol through azeotropic distillation column about by methyl alcohol and iso-butylene synthetic.
Methyl tertiary butyl ether is called for short MTBE, and it is the ideal blending component that improves gasoline octane rating, regulates the gasoline oxygen level, is again to produce the important source material of isoprene-isobutylene rubber with high-purity iso-butylene.Divide by purposes, the title of oil refining type and chemical industry type MTBE is often arranged.The finished product index of chemical industry type MTBE is to methyl sec-butyl ether (being called for short MSBE) and total carbon four C
4, trimethyl carbinol TBA, oligopolymer LP, methyl alcohol CH
3Foreign matter contents such as OH all have strict requirement.Concrete finished product index is by weight percentage: MTBE＞99%, MSBE＜0.1%, C
4＜0.01%, CH
3OH＜0.1%, TBA＜0.1%, LP＜0.1%, moisture content: no free-water.MSBE in these indexs is owing to be the isomer of MTBE, and its boiling point and MTBE are very approaching, is difficult to remove by distillating method, needs to solve by process optimization.All the other indexs all can be removed by rectifying.When separating these polynary components, usually need a lot of towers to separate in the past, both need expend a lot of facility investments, expended lot of energy simultaneously.Disclose the technology of a kind of MTBE of preparation in the U.S. Pat 3979461, but that its MTBE does not continue behind the component distillation column distillation is refining, thereby is difficult to obtain purer, meet the MTBE of chemical industry type requirement.Document EP 0535918A
1Introduced the purge process of MTBE, it is to have added 10～30% water in the rectifying raw material.Increase the load of separator column like this, and needed multistep to remove other component.Document EP 0629601A
1In introduced the technology of producing MTBE, the rectifying in the document is to adopt conventional technology, needs to separate through multitower to obtain the MTBE product.In order to overcome the shortcoming that refining energy is too many, facility investment is big of MTBE in the present production, provide a kind of in the MTBE production process, saving energy, less investment, can separate light, heavy component by single tower, simultaneously can obtain to meet the MTBE process for refining of chemical industry type MTBE ingredient requirement again, we have invented a kind of methyl tertiary butyl ether purified novel method.
The objective of the invention is to realize: methyl alcohol and iso-butylene synthetic by following technical scheme, removed the thick methyl tertiary butyl ether of most of carbon four and methyl alcohol through azeotropic distillation column, in same rectifying tower, separate the weight component simultaneously, and the methyl tertiary butyl ether that obtains refining with liquid phase side cut form.
Removed the rectifying tower that thick MTBE behind most residue carbon four and the methyl alcohol enters 15～50 blocks of column plates in the foregoing invention, total preferably stage number is 20～30 blocks of column plates.Rectifying Tata still temperature is that 80～150 ℃, tower top temperature are 45～65 ℃.The working pressure of tower is normal pressure to 5 normal atmosphere, cat head material partial reflux; Or the mode of employing total reflux, reflux ratio is 1.0～4.0, is preferably 2.0～3.0.The thick MTBE of raw material has an openning of drawing the liquid phase side cut by intermediate feed at least in the position of rectifying tower column plate sum 1/3～2/3.Its light component C
4Deng toward the cat head enrichment, collect phlegma with the condensation way, phlegma refluxes, and the non-condensable gas discharging is removed.A large amount of MTBE extract the material mode by middle openning out with liquid phase and are collected, and its component content meets the ingredient requirement of chemical industry type MTBE fully.Heavy component TBA, LP etc. are separated toward the enrichment of tower still.
The present invention makes thick MTBE finish the separation of weight component by single tower owing to adopted the technology of liquid phase side line extraction fraction, and has obtained to meet the chemical industry type MTBE of preparation high-purity isobutylene ingredient requirement.Draw in the MTBE component by weight percentage: MTBE＞99%, MSBE＜0.1%, C
4＜0.01%, CH
3OH＜0.1%, TBA＜0.3%, LP＜0.1%, H
2O: no free-water.This technology had both been saved further isolating equipment in the conventional separation, had saved further isolating energy consumption simultaneously, had realized that single tower separates the effect of weight component simultaneously.
[embodiment 1]
By the MTBE that methyl alcohol and iso-butylene obtain through certain processing condition control, elder generation is through the component distillation column distillation.Removed the thick MTBE behind most residue carbon four and the methyl alcohol, its composition is by weight percentage: total C
4: CH 0.12%,
3COH:0.094%, MTBE:98.3%, MSBE:0.075%, ETBE:0.05%, TBA:0.53%, LP:0.3%, X
1-5Carbon pentaether class: 0.06%.This thick MTBE is pumped into an internal diameter with 300ml/hr after cummulative metering be in the stuffing rectification column of 40mm.Total stage number of this rectifying tower is 18, and the opening for feed position is at the 5th column plate place, and the rectifying tower top material partly refluxes, and reflux ratio is 3.5.Tower still temperature is 100 ℃, and tower top temperature is 50 ℃.Sentence liquid phase side line extraction material mode at the 9th block of column plate and extract the qualified MTBE product that refines out, its composition is MTBE:99.4%, MSBE:0.074%, total C by weight percentage
4: 50ppm, CH
3OH:250ppm, TBA:600ppm, LP:120ppm, ETBE:80ppm, X
1-55Carbon pentaether class: 50ppm, the MTBE rate of recovery of extracting the material mode through the liquid phase side line out is 99.6%.[embodiment 2]
Each step and thick MTBE charging according to embodiment 1, total stage number of this rectifying tower is 23, the opening for feed position is at the 6th column plate place, rectifying tower top material partial reflux, reflux ratio is 2.5, tower still temperature is 120 ℃, and tower top temperature is 52 ℃, sentences liquid phase side line extraction material mode at the 13rd block of column plate and extracts the qualified MTBE product that refines out.Its composition is by weight percentage: MTBE:99.5%, MSBE:0.075%, total C
4: 40ppm, CH
3OH:230ppm, TBA:500ppm, LP:110ppm, ETBE:80ppm, X
1-5Carbon pentaether class: 50ppm, the MTBE rate of recovery of extracting the material mode through the liquid phase side line out is 99.7%.[embodiment 3]
Each step and thick MTBE charging according to embodiment 1, total stage number of this rectifying tower is 30, the opening for feed position is at the 7th column plate place, rectifying tower top material partial reflux, reflux ratio is 2.0, tower still temperature is 130 ℃, and tower top temperature is 53 ℃, sentences liquid phase side line extraction material mode at the 14th block of column plate and extracts the qualified MTBE product that refines out.Its composition is by weight percentage: MTBE:99.6%, MSBE:0.073%, total C
4: 40ppm, CH
3OH:200ppm, TBA:450ppm, LP:100ppm, ETBE:81ppm, X
1-5Carbon pentaether class: 48ppm, the MTBE rate of recovery of extracting the material mode through the liquid phase side line out is 99.7%.[embodiment 4]
Each step and thick MTBE charging according to embodiment 1, total stage number of this rectifying tower is 45, the opening for feed position is at the 8th column plate place, rectifying tower top material partial reflux, reflux ratio is 1.5, tower still temperature is 150 ℃, and tower top temperature is 55 ℃, sentences liquid phase side line extraction material mode at the 27th block of column plate and extracts the qualified MTBE product that refines out.Its composition is by weight percentage: MTBE:99.4%, MSBE:0.074%, total C
4: 30ppm, CH
3OH:180ppm, TBA:400ppm, LP:95ppm, ETBE:75ppm, X
1-5Carbon pentaether class: 46ppm, the MTBE rate of recovery of extracting the material mode through the liquid phase side line out is 99.6%.
Claims (4)
1. one kind by methyl alcohol and iso-butylene synthetic, removed the process for purification of the thick methyl tertiary butyl ether of most of carbon four and methyl alcohol through azeotropic distillation column, it is characterized in that in same rectifying tower, separating simultaneously light, heavy component, and the methyl tertiary butyl ether that obtains refining with liquid phase side cut form in the position of total stage number 1/3rd to 2/3rds, wherein total stage number of rectifying tower is 15～50, the tower still temperature of rectifying tower is 80～150 ℃, tower top temperature is 45～65 ℃, the light component partial reflux that cat head steams, reflux ratio is 1.0～4.0; Or employing total reflux mode.
2. according to the process for purification of the described thick methyl tertiary butyl ether of claim 1, it is characterized in that the outlet of drawing the liquid phase side cut is at least 1.
3. according to the process for purification of the described thick methyl tertiary butyl ether of claim 1, the reflux ratio that it is characterized in that the cat head partial reflux is 2.0～3.0; Or employing total reflux mode.
4. according to the process for purification of the described thick methyl tertiary butyl ether of claim 1, the total stage number that it is characterized in that rectifying tower is 20～30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95113371A CN1045430C (en) | 1995-12-26 | 1995-12-26 | Technique for refining methyl t-butyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95113371A CN1045430C (en) | 1995-12-26 | 1995-12-26 | Technique for refining methyl t-butyl ether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1153162A CN1153162A (en) | 1997-07-02 |
| CN1045430C true CN1045430C (en) | 1999-10-06 |
Family
ID=5079982
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95113371A Expired - Lifetime CN1045430C (en) | 1995-12-26 | 1995-12-26 | Technique for refining methyl t-butyl ether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045430C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781282B (en) * | 2010-01-28 | 2013-04-03 | 安徽时联特种溶剂股份有限公司 | Method for producing high-purity ether used for HPLC |
| CN107382681A (en) * | 2017-08-01 | 2017-11-24 | 山东滨庆新能源开发有限公司 | After the washing of MTBE devices methanol after ether carbon four into azeotropy rectification column reflux technique |
| CN107337590A (en) * | 2017-08-29 | 2017-11-10 | 湖北工程学院 | Chromatographically pure t-butyl methyl ether and preparation method thereof, production system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0535918A1 (en) * | 1991-10-03 | 1993-04-07 | Texaco Chemical Company | Purification of methyl tertiary-butyl ether |
| CN1094026A (en) * | 1992-12-30 | 1994-10-26 | 菲利浦石油公司 | The recovery of ether |
-
1995
- 1995-12-26 CN CN95113371A patent/CN1045430C/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0535918A1 (en) * | 1991-10-03 | 1993-04-07 | Texaco Chemical Company | Purification of methyl tertiary-butyl ether |
| CN1094026A (en) * | 1992-12-30 | 1994-10-26 | 菲利浦石油公司 | The recovery of ether |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1153162A (en) | 1997-07-02 |
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Granted publication date: 19991006 |
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