CN105085198A - Purification method of chromatographic grade methyl tert-butyl ether - Google Patents
Purification method of chromatographic grade methyl tert-butyl ether Download PDFInfo
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- CN105085198A CN105085198A CN201410209223.9A CN201410209223A CN105085198A CN 105085198 A CN105085198 A CN 105085198A CN 201410209223 A CN201410209223 A CN 201410209223A CN 105085198 A CN105085198 A CN 105085198A
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- butyl ether
- tertiary butyl
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Abstract
The invention discloses a purification method of chromatographic grade methyl tert-butyl ether. The method is characterized in that impurities in a raw material, methyl tert-butyl ether, are removed through processes such as modified active carbon adsorption and the like so as to obtain the chromatographic grade methyl tert-butyl ether. By the purification method of chromatographic grade methyl tert-butyl ether, methyl tert-butyl ether with purity being greater than or equal to 99.99 wt% can be obtained. The method meets high-purity requirement of a chromatographic grade reagent. Therefore, methyl tert-butyl ether obtained after purification can be applied in fields of chromatographic analysis, chromatographic separation, chromatographic preparation and the like, and the application range of methyl tert-butyl ether is broadened.
Description
Technical field
The present invention relates to solvent purification field, particularly a kind of method of purification of chromatographic grade methyl tertiary butyl ether.
Background technology
Chromatorgaphy reagent refers to the chemical reagent prepared for stratographic analysis, chromatographic separation, chromatogram.Because chromatogram kind is many, process is complicated, therefore again chromatorgaphy reagent is categorized into various different chromatorgaphy reagent as gas-chromatography reagent, high pressure liquid chromatography reagent, reagent for thin-layer chromatography, column chromatography chromatogram reagent, chromatography of ions reagent, Ion-pair chromalography reagent etc.Methyl tertiary butyl ether, as a kind of excellent liquid chromatography reagent, is applied to the aspects such as efficient liquid phase chromatographic analysis.
The preparation method of China's methyl tertiary butyl ether liquid chromatography reagent seldom has report, and domestic methyl tertiary butyl ether generally adopts methyl alcohol and iso-butylene to be raw material, and the effect by an acidic catalyst is synthesized.The methyl tertbutyl ether yield obtained by aforesaid method is lower, and containing impurity such as olefines, alcohols, water, purity is not high.The most dependence on import of high-purity methyl tertbutyl ether, causes cost higher, pins down degree larger by foreign technology.So the method developing the purification of a kind of methyl tertiary butyl ether is particularly urgent.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, a kind of method of purification improving the chromatographic grade methyl tertiary butyl ether of methyl tertiary butyl ether purity is provided.
For realizing above object, the present invention is achieved through the following technical solutions:
The method of purification of chromatographic grade methyl tertiary butyl ether, is characterized in that, comprises the steps:
A. raw material methyl tertiary butyl ether is got, add alkali metal compound wherein, as carbonate (including but not limited to sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus), alkalimetal oxide (including but not limited to sodium oxide) or alkali metal hydroxide (including but not limited to sodium hydroxide), pH value is adjusted in the scope of 7 ~ 8; Jolting, makes the acidic impurities in alkalimetal oxide, alkali metal hydroxide or carbonate and raw material methyl tertiary butyl ether fully react, production precipitation of salts thing; After stratification, discard water layer, and the organic layer being dissolved with methyl tertiary butyl ether is filtered, retain filtrate.
B. sorbent material post filtrate the passing into of step a gained being equipped with modified activated carbon carries out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds, obtains the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
Preferably, methyl tertiary butyl ether with 0.5-30 column volume/hour speed flow through the sorbent material post that modified activated carbon is housed.
Preferably, described modified activated carbon is the activated carbon of surface attachment oxidizing acid solution.The particle diameter of activated carbon is 20 ~ 100 orders.The volumetric concentration of oxidizing acid solution is 5% ~ 60%.Described oxidizing acid includes but not limited to concentrated nitric acid, dust technology, the vitriol oil, hypochlorous acid, chloric acid, chlorous acid, perchloric acid, nitrous acid.
Preferably, in described step b, before filtrate passing into is equipped with the sorbent material post of modified activated carbon, first passes into and the sorbent material post that particle diameter is 20 ~ 100 orders, model is the molecular sieve of 3A or 4A is housed, remove moisture.
Preferably, methyl tertiary butyl ether with 0.5 ~ 30 column volume/hour speed flow through the sorbent material post that molecular sieve is housed.
Preferably, in described step b, the methyl tertiary butyl ether after modified active carbon adsorption is passed into the sorbent material post that particle diameter is 20 ~ 200 object aluminum oxide is housed, remove the impurity such as alcohols.
Preferably, methyl tertiary butyl ether with 0.5 ~ 30 column volume/hour speed flow through the sorbent material post that aluminum oxide is housed.
Preferably, also comprise step c, the methyl tertiary butyl ether after absorption is carried out rectifying.
Preferably, rectifying still Heating temperature is 83 ~ 95 DEG C, methyl tertiary butyl ether fluid temperature is 83 ~ 86 DEG C, goes out liquid temp and be 55 ~ 56 DEG C, control reflux ratio 20: 1 ~ 10:1, total reflux 1 ~ 3 hour in still.
The method of purification of chromatographic grade methyl tertiary butyl ether provided by the invention, the methyl tertiary butyl ether of purity >=99.99% (wt) is obtained by modified active carbon adsorption, the field such as the methyl tertiary butyl ether that purification is obtained is applied to stratographic analysis, prepared by chromatographic separation, chromatogram, expands range of application.Method of purification provided by the invention, the production having filled up domestic high-purity methyl tertbutyl ether is blank, reduces cost needed for import, alleviates the degree pind down by foreign technology simultaneously.Method of purification provided by the invention, product yield >=95%, yield is high, also have that energy consumption is low, production process is easy simultaneously, stable, be applicable to the advantages such as suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail:
Embodiment 1
The method of purification of chromatographic grade methyl tertiary butyl ether, comprises the steps:
A. get the raw material methyl tertiary butyl ether that purity is 99.5% (wt), add sodium carbonate by the pH regulator to 7 of solution, and jolting makes the acidic impurities in sodium carbonate and raw material methyl tertiary butyl ether fully react, generate precipitation of salts thing; Stratification, discards water layer and precipitation, filters organic layer, retains filtrate.
B. adsorb:
I. by above-mentioned filtrate with 0.5 column volume/hour speed pass into the sorbent material post that particle diameter is 50 object 3A molecular sieves be housed, remove the moisture in organic layer further; After absorption, methyl tertiary butyl ether water content control is ≤0.03%; Utilize molecular sieve to remove moisture after extraction in methyl tertiary butyl ether in this step, as moisture content > 0.03% need change molecular sieve after proceed molecular sieve adsorption process again;
II. and then, by above-mentioned effluent liquid with 20 column volumes/hour speed pass into the sorbent material post that modified activated carbon is housed, modified activated carbon is the particle diameter that the nitric acid dousing being 60% through volumetric concentration is crossed is 100 object activated carbon, for removing the organic compound of carbon-carbon double bonds, as olefines impurity; Due to the group that carbon-carbon double bond is Absorbable rod ultraviolet-visible, so remove the transparence that the organic compound of carbon-carbon double bonds can improve the methyl tertiary butyl ether after purification greatly;
III. last, by above-mentioned effluent liquid with 10 column volumes/hour speed pass into and the sorbent material post that particle diameter is 200 object aluminum oxide be housed, for removing alcohols impurity.
C. above-mentioned methyl tertiary butyl ether after adsorption treatment is squeezed into rectifying tower and carry out rectifying, obtain the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
Rectifying can adopt known manner to carry out.A kind of optimal way of the present invention is, rectifying still Heating temperature is 95 DEG C, methyl tertiary butyl ether fluid temperature is 85 DEG C in still, to go out liquid temp be 55 DEG C, reflux ratio 12: 1, total reflux 3 hours.Rectifying fluid detects qualified rear bottling, and inflated with nitrogen is preserved,
Embodiment 2
The method of purification of chromatographic grade methyl tertiary butyl ether, comprises the steps:
A. get the raw material methyl tertiary butyl ether that purity is 99.5% (wt), add potassium hydroxide by the pH regulator to 8 of solution, and jolting makes the acidic impurities in potassium hydroxide and raw material methyl tertiary butyl ether fully react, generate precipitation of salts thing; Stratification, discards water layer and precipitation, filters organic layer, retains filtrate.
B. adsorb:
I. by above-mentioned filtrate with 30 column volumes/hour speed pass into the sorbent material post that particle diameter is 20 object 3A molecular sieves be housed, remove the moisture in organic layer further; After absorption, methyl tertiary butyl ether water content control is ≤0.03%; Utilize molecular sieve to remove moisture after extraction in methyl tertiary butyl ether in this step, as moisture content > 0.03% need change molecular sieve after proceed molecular sieve adsorption process again;
II. and then, by above-mentioned effluent liquid with 6 column volumes/hour speed pass into the sorbent material post that modified activated carbon is housed, modified activated carbon is the particle diameter that the sulfuric acid being 60% through volumetric concentration soaked is 80 object activated carbon, for removing the organic compound of carbon-carbon double bonds, as olefines impurity; Due to the group that carbon-carbon double bond is Absorbable rod ultraviolet-visible, so remove the transparence that the organic compound of carbon-carbon double bonds can improve the methyl tertiary butyl ether after purification greatly;
III. last, by above-mentioned effluent liquid with 0.5 column volume/hour speed pass into and the sorbent material post that particle diameter is 100 object aluminum oxide be housed, for removing alcohols impurity.
C. above-mentioned methyl tertiary butyl ether after adsorption treatment is squeezed into rectifying tower and carry out rectifying, obtain the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
Rectifying can adopt known manner to carry out.A kind of optimal way of the present invention is, rectifying still Heating temperature is 83 DEG C, methyl tertiary butyl ether fluid temperature is 83 DEG C in still, to go out liquid temp be 55.5 reflux ratios 10: 1 processed, total reflux 1 hour.By controlling out liquid temp.Rectifying fluid detects qualified rear bottling, and inflated with nitrogen is preserved.
Embodiment 3
The method of purification of chromatographic grade methyl tertiary butyl ether, comprises the steps:
A. get the raw material methyl tertiary butyl ether that purity is 99.5% (wt), add sodium oxide by the pH regulator to 7.5 of solution, and jolting makes the acidic impurities in sodium oxide and raw material methyl tertiary butyl ether fully react, generate precipitation of salts thing; Stratification, discards water layer and precipitation, filters organic layer, retains filtrate.
B. adsorb:
I. by above-mentioned filtrate with 15 column volumes/hour speed pass into the sorbent material post that particle diameter is 100 order molecular sieves be housed, remove the moisture in organic layer further; After absorption, methyl tertiary butyl ether water content control is ≤0.03%; Utilize molecular sieve to remove moisture after extraction in methyl tertiary butyl ether in this step, as moisture content > 0.03% need change molecular sieve after proceed molecular sieve adsorption process again;
II. and then, by above-mentioned effluent liquid with 0.5 column volume/hour speed pass into the sorbent material post that modified activated carbon is housed, modified activated carbon is the particle diameter that the hypochlorous acid being 5% through volumetric concentration soaked is 20 object activated carbon, for removing the organic compound of carbon-carbon double bonds, as olefines impurity; Due to the group that carbon-carbon double bond is Absorbable rod ultraviolet-visible, so remove the transparence that the organic compound of carbon-carbon double bonds can improve the methyl tertiary butyl ether after purification greatly;
III. last, by above-mentioned effluent liquid with 30 column volumes/hour speed pass into and the sorbent material post that particle diameter is 20 object aluminum oxide be housed, for removing alcohols impurity.
C. above-mentioned methyl tertiary butyl ether after adsorption treatment is squeezed into rectifying tower and carry out rectifying, obtain the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
Rectifying can adopt known manner to carry out.A kind of optimal way of the present invention is, rectifying still Heating temperature is 90 DEG C, methyl tertiary butyl ether fluid temperature is 86 DEG C, goes out liquid temp and be 56, control reflux ratio 20: 1, total reflux 2 hours in still.Rectifying fluid detects qualified rear bottling, and inflated with nitrogen is preserved.
Embodiment 4
The method of purification of chromatographic grade methyl tertiary butyl ether, comprises the steps:
A. get the raw material methyl tertiary butyl ether that purity is 99.5% (wt), add potassium hydroxide by the pH regulator to 8 of solution, and jolting makes the acidic impurities in potassium hydroxide and raw material methyl tertiary butyl ether fully react, generate precipitation of salts thing; Stratification, discards water layer and precipitation, filters organic layer, retains filtrate.
B. adsorb:
I. by above-mentioned filtrate with 24 column volumes/hour speed pass into the sorbent material post that particle diameter is 65 molecules of interest sieves be housed, remove further the moisture in organic layer; After absorption, methyl tertiary butyl ether water content control is ≤0.03%; Utilize molecular sieve to remove moisture after extraction in methyl tertiary butyl ether in this step, as moisture content > 0.03% need change molecular sieve after proceed molecular sieve adsorption process again;
II. and then, by above-mentioned effluent liquid with 30 column volumes/hour speed pass into the sorbent material post that modified activated carbon is housed, modified activated carbon is the particle diameter that the perchloric acid being 45% through volumetric concentration soaked is 45 object activated carbon, for removing the organic compound of carbon-carbon double bonds, as olefines impurity; Due to the group that carbon-carbon double bond is Absorbable rod ultraviolet-visible, so remove the transparence that the organic compound of carbon-carbon double bonds can improve the methyl tertiary butyl ether after purification greatly;
III. last, by above-mentioned effluent liquid with 16 column volumes/hour speed pass into and the sorbent material post that particle diameter is 135 object aluminum oxide be housed, for removing alcohols impurity.
C. above-mentioned methyl tertiary butyl ether after adsorption treatment is squeezed into rectifying tower and carry out rectifying, obtain the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
Rectifying can adopt known manner to carry out.A kind of optimal way of the present invention is, rectifying still Heating temperature is 96 DEG C, methyl tertiary butyl ether fluid temperature is 86 DEG C in still, to go out liquid temp be 55.5 reflux ratios 19: 1 processed, total reflux 2.5 hours.Rectifying fluid detects qualified rear bottling, and inflated with nitrogen is preserved.
Embodiment 1 ~ 4 purify after chromatographic grade methyl tertiary butyl ether technical indicator as shown in Table 1:
Table one
As shown in Table 1, by the chromatographic grade methyl tertiary butyl ether comparatively raw material methyl tertiary butyl ether that method of purification provided by the invention is obtained, to wavelength be the incident light of 207nm, 217nm, 232nm, 242nm and 260nm transmittance comparatively raw material also greatly improve, improve the optical property of chromatographic grade methyl tertiary butyl ether.Especially be that the transparence of the incident light of 260nm reaches more than 98% to wavelength.Purity promotes further, and water content also reduces greatly.Meanwhile, the yield of the chromatographic grade methyl tertiary butyl ether that the method for purification improved by the present invention is obtained all is not less than 95%, can cut the waste, and reduces production cost.
Embodiment in the present invention, only for the present invention will be described, does not form the restriction to right, other equivalent in fact substituting, all in scope that those skilled in that art can expect.
Claims (9)
1. the method for purification of chromatographic grade methyl tertiary butyl ether, is characterized in that, comprises the steps:
A. get raw material methyl tertiary butyl ether, add alkalimetal oxide, alkali metal hydroxide or carbonate wherein, after jolting, stratification, discard water layer, filter organic layer, retain filtrate;
B. sorbent material post filtrate the passing into of step a gained being equipped with modified activated carbon carries out adsorption treatment, obtains the chromatographic grade methyl tertiary butyl ether of purity >=99.99% (wt).
2. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 1, is characterized in that, in described step b, liquid with 0.5 ~ 30 column volume/hour speed flow through the sorbent material post that modified activated carbon is housed.
3. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 1, is characterized in that, described alkali metal compound comprises an alkali metal salt, alkalimetal oxide and alkali metal hydroxide.
4. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 1, is characterized in that, described modified activated carbon is the activated carbon of surface attachment oxidizing acid.
5. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 1, is characterized in that, in described step b, before filtrate passing into is equipped with the sorbent material post of modified activated carbon, first passes into the sorbent material post that molecular sieve is housed.
6. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 5, is characterized in that, liquid with 0.5 ~ 30 column volume/hour speed flow through the sorbent material post that molecular sieve is housed.
7. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 1, is characterized in that, in described step b, the methyl tertiary butyl ether after modified active carbon adsorption is passed into the sorbent material post that aluminum oxide is housed.
8. the method for purification of chromatographic grade methyl tertiary butyl ether according to claim 7, is characterized in that, liquid with 0.5 ~ 30 column volume/hour speed flow through the sorbent material post that aluminum oxide is housed.
9. according to the method for purification of the chromatographic grade methyl tertiary butyl ether above described in arbitrary claim, it is characterized in that, also comprise step c, the methyl tertiary butyl ether after absorption is carried out rectifying.
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Cited By (5)
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| CN105198858A (en) * | 2015-10-30 | 2015-12-30 | 天津药物研究院药业有限责任公司 | Purification method of zaltoprofen |
| CN106349029A (en) * | 2016-08-29 | 2017-01-25 | 国药集团化学试剂有限公司 | Preparation method of chromatographic-grade methyl tert-butyl ether |
| CN109384653A (en) * | 2017-08-02 | 2019-02-26 | 中国石油化工股份有限公司 | High-purity MTBE production technology |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198858A (en) * | 2015-10-30 | 2015-12-30 | 天津药物研究院药业有限责任公司 | Purification method of zaltoprofen |
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| 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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