CN105085198B - The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE) - Google Patents
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE) Download PDFInfo
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- CN105085198B CN105085198B CN201410209223.9A CN201410209223A CN105085198B CN 105085198 B CN105085198 B CN 105085198B CN 201410209223 A CN201410209223 A CN 201410209223A CN 105085198 B CN105085198 B CN 105085198B
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- mtbe
- butyl ether
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Abstract
The invention discloses a kind of method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), it is characterised in that removes the impurity in raw material methyl tertiary butyl ether(MTBE) by processes such as modified active carbon adsorptions, obtains chromatographic grade methyl tertiary butyl ether(MTBE).The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE) provided by the invention, it can obtain purity >=99.99% (wt) methyl tertiary butyl ether(MTBE), meet the high-purity requirement of chromatographic grade reagent, the methyl tertiary butyl ether(MTBE) for enabling purification to obtain is applied to the fields such as chromatography, chromatographic isolation, chromatogram preparation, expands application.
Description
Technical field
The present invention relates to solvent purifications field, more particularly to a kind of method of purification of chromatographic grade methyl tertiary butyl ether(MTBE).
Background technology
Chromatorgaphy reagent refers to the chemical reagent prepared for chromatography, chromatographic isolation, chromatogram.Because chromatogram species is more, mistake
Journey is complicated, therefore chromatorgaphy reagent is categorized into a variety of chromatorgaphy reagents such as again：Gas-chromatography reagent, high pressure liquid chromatography examination
Agent, reagent for thin-layer chromatography, column chromatography chromatogram reagent, chromatography of ions reagent, Ion-pair chromalography reagent etc..Methyl tertiary butyl ether(MTBE) conduct
A kind of excellent liquid chromatogram reagent, applied to efficient liquid phase chromatographic analysis etc..
The preparation method of China's methyl tertiary butyl ether(MTBE) liquid chromatogram reagent seldom has been reported that, domestic methyl tertiary butyl ether(MTBE) one
As use methanol and isobutene as raw material, by acidic catalyst effect synthesize.Pass through methyl- tert fourth made from the above method
Base ether yield is relatively low, and not high containing impurity, purity such as olefines, alcohols, water.High-purity methyl tertbutyl ether rely on mostly into
Mouthful, cause cost higher, it is larger to be pind down degree by foreign technology.So it is outstanding to develop a kind of method of methyl tertiary butyl ether(MTBE) purification
To be urgent.
The content of the invention
The invention aims to overcome deficiency of the prior art, there is provided one kind can improve methyl tertiary butyl ether(MTBE) purity
Chromatographic grade methyl tertiary butyl ether(MTBE) method of purification.
To realize object above, the present invention is achieved through the following technical solutions：
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), it is characterised in that comprise the following steps：
A. raw material methyl tertiary butyl ether(MTBE) is taken, adds alkali metal compound thereto, as carbonate (includes but is not limited to carbonic acid
Sodium, sodium acid carbonate, potassium carbonate, saleratus), alkali metal oxide (include but is not limited to sodium oxide molybdena) or alkali metal hydroxide
(including but is not limited to sodium hydroxide), pH value is adjusted in the range of 7~8；Shaking, makes alkali metal oxide, alkali metal hydrogen
Oxide or carbonate fully react with the acid impurities in raw material methyl tertiary butyl ether(MTBE), produce precipitation of salts thing；Stratification
Afterwards, water layer is discarded, and the organic layer dissolved with methyl tertiary butyl ether(MTBE) is filtered, retains filtrate.
B. the filtrate obtained by step a is passed through the adsorbent post equipped with modified activated carbon and carries out adsorption treatment, for removing
The unsaturated organic compound of carbon-carbon double bonds, obtain the chromatographic grade methyl tertiary butyl ether(MTBE) of purity >=99.99% (wt).
Preferably, methyl tertiary butyl ether(MTBE) flows through the suction equipped with modified activated carbon with the speed of 0.5-30 column volumes/hour
Attached dose of post.
Preferably, the modified activated carbon is the activated carbon of surface attachment oxidizing acid solution.The particle diameter of activated carbon is
20~100 mesh.The volumetric concentration of oxidizing acid solution is 5%~60%.The oxidizing acid includes but is not limited to concentrated nitric acid, dilute
Nitric acid, the concentrated sulfuric acid, hypochlorous acid, chloric acid, chlorous acid, perchloric acid, nitrous acid.
Preferably, in the step b, filtrate is passed through before the adsorbent post equipped with modified activated carbon, is first passed through and is equipped with
Particle diameter is 20~100 mesh, the adsorbent post of model 3A or 4A molecular sieve, removes moisture removal.
Preferably, methyl tertiary butyl ether(MTBE) flows through the adsorbent equipped with molecular sieve with the speed of 0.5~30 column volume/hour
Post.
Preferably, in the step b, the methyl tertiary butyl ether(MTBE) after modified active carbon adsorption is passed through it is equipped with particle diameter
The adsorbent post of the aluminum oxide of 20~200 mesh, remove the impurity such as alcohols.
Preferably, methyl tertiary butyl ether(MTBE) flows through the adsorbent equipped with aluminum oxide with the speed of 0.5~30 column volume/hour
Post.
Preferably, in addition to step c, the methyl tertiary butyl ether(MTBE) after absorption is subjected to rectifying.
Preferably, rectifying still heating-up temperature be 83~95 DEG C, in kettle methyl tertiary butyl ether(MTBE) fluid temperature be 83~86 DEG C,
Go out liquid temperature degree for 55~56 DEG C, control reflux ratio 20: 1~10:1st, infinite reflux 1~3 hour.
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE) provided by the invention, by modified active carbon adsorption obtain purity >=
99.99% (wt) methyl tertiary butyl ether(MTBE), the methyl tertiary butyl ether(MTBE) for enabling purification to obtain are applied to chromatography, chromatogram point
The field such as prepare from, chromatogram, expand application.Method of purification provided by the invention, domestic high-purity methyl uncle is filled up
The production blank of butyl ether, reduces cost needed for import, while alleviates the degree pind down by foreign technology.The present invention provides
Method of purification, product yield >=95%, high income, while also have energy consumption is low, production process is easy, stable, applicable
In the industrialized production the advantages that.
Embodiment
The present invention is described in detail with reference to embodiment：
Embodiment 1
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), comprises the following steps：
A. the raw material methyl tertiary butyl ether(MTBE) that purity is 99.5% (wt) is taken, sodium carbonate is added and adjusts the pH of solution to 7, and
Shaking makes sodium carbonate fully be reacted with the acid impurities in raw material methyl tertiary butyl ether(MTBE), generates precipitation of salts thing；Stratification, abandon
Water layer and precipitation are gone, filters organic layer, retains filtrate.
B. adsorb：
I., above-mentioned filtrate is passed through to the absorption equipped with particle diameter as the 3A molecular sieves of 50 mesh using the speed of 0.5 column volume/hour
Agent post, further remove the moisture in organic layer；After absorption, methyl tertiary butyl ether(MTBE) water content control is ≤0.03%；This step
The middle moisture removed using molecular sieve after extraction in methyl tertiary butyl ether(MTBE), after need to changing molecular sieve such as moisture ＞ 0.03%
It is further continued for carrying out molecular sieve adsorption processing；
II. and then, above-mentioned efflux is passed through the adsorbent equipped with modified activated carbon with the speed of 20 column volumes/hour
Post, modified activated carbon is the activated carbon that the particle diameter that the nitric acid dousing for being 60% through volumetric concentration is crossed is 100 mesh, carbon containing for removing
The organic compound of carbon double bond, such as olefines impurity；Because carbon-carbon double bond is the group of absorbable ultraviolet-visible, so removing
The organic compound of carbon-carbon double bonds is greatly improved the light transmittance of the methyl tertiary butyl ether(MTBE) after purification；
III. finally, above-mentioned efflux is passed through to the aluminum oxide equipped with particle diameter as 200 mesh using the speed of 10 column volumes/hour
Adsorbent post, for removing alcohols impurity.
C. by the above-mentioned methyl tertiary butyl ether(MTBE) after adsorption treatment squeeze into rectifying column carry out rectifying, produce purity >=
99.99% (wt) chromatographic grade methyl tertiary butyl ether(MTBE).
Rectifying can use known manner to carry out.A kind of preferred embodiment of the present invention is that rectifying still heating-up temperature is 95 DEG C, kettle
It is 55 DEG C that middle methyl tertiary butyl ether(MTBE) fluid temperature, which is 85 DEG C, goes out liquid temperature degree, reflux ratio 12: 1, infinite reflux 3 hours.Smart distillate inspection
Qualified rear bottling is surveyed, inflated with nitrogen preserves,
Embodiment 2
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), comprises the following steps：
A. the raw material methyl tertiary butyl ether(MTBE) that purity is 99.5% (wt) is taken, potassium hydroxide is added and adjusts the pH of solution to 8,
And shaking makes potassium hydroxide fully be reacted with the acid impurities in raw material methyl tertiary butyl ether(MTBE), precipitation of salts thing is generated；Stand and divide
Layer, water layer and precipitation are discarded, filter organic layer, retain filtrate.
B. adsorb：
I., above-mentioned filtrate is passed through to the adsorbent equipped with particle diameter as the 3A molecular sieves of 20 mesh using the speed of 30 column volumes/hour
Post, further remove the moisture in organic layer；After absorption, methyl tertiary butyl ether(MTBE) water content control is ≤0.03%；In this step
Moisture after extraction in methyl tertiary butyl ether(MTBE) is removed using molecular sieve, as moisture ＞ 0.03% need to be changed after molecular sieve again
Continue molecular sieve adsorption processing；
II. and then, above-mentioned efflux is passed through the adsorbent equipped with modified activated carbon with the speed of 6 column volumes/hour
Post, modified activated carbon is the activated carbon that the particle diameter that the sulfuric acid for being 60% through volumetric concentration soaked is 80 mesh, carbon containing for removing
The organic compound of carbon double bond, such as olefines impurity；Because carbon-carbon double bond is the group of absorbable ultraviolet-visible, so removing
The organic compound of carbon-carbon double bonds is greatly improved the light transmittance of the methyl tertiary butyl ether(MTBE) after purification；
III. finally, above-mentioned efflux is passed through to the oxidation equipped with particle diameter as 100 mesh using the speed of 0.5 column volume/hour
The adsorbent post of aluminium, for removing alcohols impurity.
C. by the above-mentioned methyl tertiary butyl ether(MTBE) after adsorption treatment squeeze into rectifying column carry out rectifying, produce purity >=
99.99% (wt) chromatographic grade methyl tertiary butyl ether(MTBE).
Rectifying can use known manner to carry out.A kind of preferred embodiment of the present invention is that rectifying still heating-up temperature is 83 DEG C, kettle
It is 55.5 reflux ratios 10: 1 processed, infinite reflux 1 hour that middle methyl tertiary butyl ether(MTBE) fluid temperature, which is 83 DEG C, goes out liquid temperature degree.Pass through control
Go out liquid temperature degree.Bottled after smart distillate detection is qualified, inflated with nitrogen preserves.
Embodiment 3
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), comprises the following steps：
A. the raw material methyl tertiary butyl ether(MTBE) that purity is 99.5% (wt) is taken, sodium oxide molybdena is added and adjusts the pH of solution to 7.5,
And shaking makes sodium oxide molybdena fully be reacted with the acid impurities in raw material methyl tertiary butyl ether(MTBE), precipitation of salts thing is generated；Stratification,
Water layer and precipitation are discarded, filters organic layer, retains filtrate.
B. adsorb：
I. above-mentioned filtrate is passed through adsorbent post equipped with particle diameter as 100 mesh molecular sieves using the speed of 15 column volumes/hour,
Further remove the moisture in organic layer；After absorption, methyl tertiary butyl ether(MTBE) water content control is ≤0.03%；Utilized in this step
Molecular sieve removes the moisture after extraction in methyl tertiary butyl ether(MTBE), is further continued for after need to changing molecular sieve such as moisture ＞ 0.03%
Carry out molecular sieve adsorption processing；
II. and then, above-mentioned efflux is passed through the absorption equipped with modified activated carbon with the speed of 0.5 column volume/hour
Agent post, modified activated carbon are the activated carbon that the particle diameter that the hypochlorous acid for being 5% through volumetric concentration soaked is 20 mesh, are contained for removing
The organic compound of carbon-carbon double bond, such as olefines impurity；Due to the group that carbon-carbon double bond is absorbable ultraviolet-visible, so going
Except the organic compound of carbon-carbon double bonds is greatly improved the light transmittance of the methyl tertiary butyl ether(MTBE) after purification；
III. finally, above-mentioned efflux is passed through to the aluminum oxide equipped with particle diameter as 20 mesh using the speed of 30 column volumes/hour
Adsorbent post, for removing alcohols impurity.
C. by the above-mentioned methyl tertiary butyl ether(MTBE) after adsorption treatment squeeze into rectifying column carry out rectifying, produce purity >=
99.99% (wt) chromatographic grade methyl tertiary butyl ether(MTBE).
Rectifying can use known manner to carry out.A kind of preferred embodiment of the present invention is that rectifying still heating-up temperature is 90 DEG C, kettle
It is 56 that middle methyl tertiary butyl ether(MTBE) fluid temperature, which is 86 DEG C, goes out liquid temperature degree, control reflux ratio 20: 1, infinite reflux 2 hours.Smart distillate
Qualified rear bottling is detected, inflated with nitrogen preserves.
Embodiment 4
The method of purification of chromatographic grade methyl tertiary butyl ether(MTBE), comprises the following steps：
A. the raw material methyl tertiary butyl ether(MTBE) that purity is 99.5% (wt) is taken, potassium hydroxide is added and adjusts the pH of solution to 8,
And shaking makes potassium hydroxide fully be reacted with the acid impurities in raw material methyl tertiary butyl ether(MTBE), precipitation of salts thing is generated；Stand and divide
Layer, water layer and precipitation are discarded, filter organic layer, retain filtrate.
B. adsorb：
I. above-mentioned filtrate is passed through the adsorbent sieved equipped with particle diameter as 65 molecules of interest using the speed of 24 column volumes/hour
Post, further remove the moisture in organic layer；After absorption, methyl tertiary butyl ether(MTBE) water content control is ≤0.03%；In this step
Moisture after extraction in methyl tertiary butyl ether(MTBE) is removed using molecular sieve, as moisture ＞ 0.03% need to be changed after molecular sieve again
Continue molecular sieve adsorption processing；
II. and then, above-mentioned efflux is passed through the adsorbent equipped with modified activated carbon with the speed of 30 column volumes/hour
Post, modified activated carbon are the activated carbon that the particle diameter that the perchloric acid for being 45% through volumetric concentration soaked is 45 mesh, are contained for removing
The organic compound of carbon-carbon double bond, such as olefines impurity；Due to the group that carbon-carbon double bond is absorbable ultraviolet-visible, so going
Except the organic compound of carbon-carbon double bonds is greatly improved the light transmittance of the methyl tertiary butyl ether(MTBE) after purification；
III. finally, above-mentioned efflux is passed through to the aluminum oxide equipped with particle diameter as 135 mesh using the speed of 16 column volumes/hour
Adsorbent post, for removing alcohols impurity.
C. by the above-mentioned methyl tertiary butyl ether(MTBE) after adsorption treatment squeeze into rectifying column carry out rectifying, produce purity >=
99.99% (wt) chromatographic grade methyl tertiary butyl ether(MTBE).
Rectifying can use known manner to carry out.A kind of preferred embodiment of the present invention is that rectifying still heating-up temperature is 96 DEG C, kettle
It is 55.5 reflux ratios 19: 1 processed, infinite reflux 2.5 hours that middle methyl tertiary butyl ether(MTBE) fluid temperature, which is 86 DEG C, goes out liquid temperature degree.Rectifying goes out
Bottled after liquid detection is qualified, inflated with nitrogen preserves.
The technical indicator of chromatographic grade methyl tertiary butyl ether(MTBE) after the purification of embodiment 1~4 is as shown in Table 1：
Table one
As shown in Table 1, by chromatographic grade methyl tertiary butyl ether(MTBE) made from method of purification provided by the invention compared with raw material methyl
Tertbutyl ether, the light transmittance for the incident light that wavelength is 207nm, 217nm, 232nm, 242nm and 260nm is also carried significantly compared with raw material
Height, improve the optical property of chromatographic grade methyl tertiary butyl ether(MTBE).Especially the light transmittance for the incident light that wavelength is 260nm is reached
More than 98%.Purity is further lifted, and water content is greatly reduced.Meanwhile by made from the method for purification of the invention improved
The yield of chromatographic grade methyl tertiary butyl ether(MTBE) is not less than 95%, can reduce waste, reduces production cost.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
Other substantially equivalent replacements that those skilled in that art are contemplated that, all fall in the scope of protection of the present invention.
Claims (4)
1. the method for purification of chromatographic grade methyl tertiary butyl ether(MTBE), it is characterised in that comprise the following steps：
A. raw material methyl tertiary butyl ether(MTBE) is taken, adds alkali metal oxide, alkali metal hydroxide or carbonate thereto, shake,
After stratification, water layer is discarded, filters organic layer, retains filtrate；
B. the filtrate obtained by step a is passed through adsorbent post equipped with modified activated carbon and carries out adsorption treatment, obtain purity >=
99.99% (wt) chromatographic grade methyl tertiary butyl ether(MTBE)；
In the step b, filtrate is passed through before the adsorbent post equipped with modified activated carbon, is first passed through the adsorbent equipped with molecular sieve
Post；
In the step b, the methyl tertiary butyl ether(MTBE) after modified active carbon adsorption is passed through to the adsorbent post equipped with aluminum oxide；
The modified activated carbon is the activated carbon of surface attachment oxidizing acid；
Also include step c, the methyl tertiary butyl ether(MTBE) after absorption is subjected to rectifying；Rectifying still heating-up temperature is 83~95 DEG C, in kettle
It is 55~56 DEG C that methyl tertiary butyl ether(MTBE) fluid temperature, which is 83~86 DEG C, goes out liquid temperature degree, control reflux ratio 20: 1~10:1st, infinite reflux
1~3 hour.
2. the method for purification of chromatographic grade methyl tertiary butyl ether(MTBE) according to claim 1, it is characterised in that in the step b,
Liquid flows through the adsorbent post equipped with modified activated carbon with the speed of 0.5~30 column volume/hour.
3. the method for purification of chromatographic grade methyl tertiary butyl ether(MTBE) according to claim 1, it is characterised in that liquid with 0.5~
The speed of 30 column volumes/hour flows through the adsorbent post equipped with molecular sieve.
4. the method for purification of chromatographic grade methyl tertiary butyl ether(MTBE) according to claim 1, it is characterised in that liquid with 0.5~
The speed of 30 column volumes/hour flows through the adsorbent post equipped with aluminum oxide.
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| CN105198858B (en) * | 2015-10-30 | 2017-07-21 | 天津药物研究院药业有限责任公司 | The purification process of Zaltoprofen |
| CN106349029B (en) * | 2016-08-29 | 2021-08-03 | 国药集团化学试剂有限公司 | Preparation method of chromatographic grade methyl tert-butyl ether |
| CN109384653B (en) * | 2017-08-02 | 2021-08-10 | 中国石油化工股份有限公司 | Production process of high-purity MTBE |
| CN109824487A (en) * | 2018-12-13 | 2019-05-31 | 天津康科德医药化工有限公司 | A kind of purification process of chromatographically pure methyl tertiary butyl ether(MTBE) |
| CN117229128A (en) * | 2023-11-13 | 2023-12-15 | 山东寿光鲁清石化有限公司 | Purification method of methyl tertiary butyl ether crude product |
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| CN1607973A (en) * | 2001-10-31 | 2005-04-20 | 霍尼韦尔国际公司 | Purification of organic solvents |
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN102924242A (en) * | 2012-08-17 | 2013-02-13 | 上海泰坦科技有限公司 | Method for purifying propylene glycol ether compounds |
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| JPH0699351B2 (en) * | 1986-04-07 | 1994-12-07 | 三井石油化学工業株式会社 | Method for producing tertiary alkyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1607973A (en) * | 2001-10-31 | 2005-04-20 | 霍尼韦尔国际公司 | Purification of organic solvents |
| CN102417441A (en) * | 2011-12-26 | 2012-04-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether |
| CN102924242A (en) * | 2012-08-17 | 2013-02-13 | 上海泰坦科技有限公司 | Method for purifying propylene glycol ether compounds |
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