CN102701920B - Method for purifying vinyl isobutyl ether - Google Patents
Method for purifying vinyl isobutyl ether Download PDFInfo
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- CN102701920B CN102701920B CN201210176295.9A CN201210176295A CN102701920B CN 102701920 B CN102701920 B CN 102701920B CN 201210176295 A CN201210176295 A CN 201210176295A CN 102701920 B CN102701920 B CN 102701920B
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- isobutyl ether
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Abstract
The invention discloses a method for purifying vinyl isobutyl ether. The method comprises the following steps of: (1) rectifying 50 to 90 mass percent of vinyl isobutyl ether solution at the temperature of between 50 and 95 DEG C under reduced pressure of between 10 and 60 kPa to obtain a distillate in which the vinyl isobutyl ether is used as a main ingredient and a kettle base solution in which isobutanol is used as a main ingredient; and (2) washing and demixing the distillate by using deionized water to obtain a superstratum organic matter and a substratum water phase, and separating the organic phase to obtain 97 to 99.5 percent of vinyl isobutyl ether. By the method, the using amount of the deionized water during washing is reduced, the washing time is saved, the production efficiency is improved, and the production cost is reduced; materials can be recycled, the discharge of waste water, waste gas and industrial residues is reduced, and environmental benefit is improved; and the quality of the product is high, and the content of the vinyl isobutyl ether is more than 98.5 percent.
Description
Technical field
The invention belongs to vinyl isobutyl ether technical field, be specifically related to a kind of method of purification of vinyl isobutyl ether.
Background technology
Vinyl isobutyl ether is colourless liquid, is easily polymerized, and dissolves in ethanol and ether, atomic water-soluble, relative density 0.7706, boiling point 83.3 DEG C, inflammable, irritant.Vinyl isobutyl ether is one of main raw material of synthesis chlorinated polyether resin, in the production process of chlorinated polyether resin, have irreplaceable effect, also can be used as the intermediate of medicine synthesis and Chemical Manufacture.
Vinyl isobutyl ether with acetylene and isopropylcarbinol for prepared by reaction raw materials, as China Patent Publication No. CN1709847A, December 21 2005 publication date, denomination of invention: the method for continuously synthesizing of vinyl isobutyl ether.This application disclose a kind of method for continuously synthesizing of vinyl isobutyl ether, it is for reaction raw materials with acetylene and isopropylcarbinol, building-up reactions is carried out in synthetic tower, the catalyst solution of 50 ~ 80% liquid levels is filled with in synthetic tower, acetylene and isobutanol gas, after nozzle mixes, synthetic tower is passed at the bottom of synthetic tower, catalyst solution at the bottom of tower continuously gets to tower top by recycle pump, circulate, synthesis etherification reaction is carried out after the acetylene small bubbles formed contact in synthetic tower with isopropylcarbinol, the temperature of etherification reaction is: 125 ~ 150 DEG C, reaction pressure 0.3 ~ the 0.6Mpa of synthetic tower, catalyzer is the isobutanol solution containing KOH, the vinyl isobutyl ether that reaction generates and unreacted acetylene, isopropylcarbinol is derived by synthetic tower tower top, receiving tank is entered after condenser, finished product vinyl isobutyl ether can be obtained again through aftertreatment.Weak point is that aftertreatment technology effect is poor, is difficult to obtain highly purified vinyl isobutyl ether.
The production technique of the vinyl isobutyl ether of existing serialization is in the purification process in later stage, often run into the problem that isopropylcarbinol and vinyl isobutyl ether exist azeotropic, therefore separation difficulty, existing technique generally adopts the method for being interrupted autoclave washing by the isopropylcarbinol removing in azeotrope, this method of purification water content consumption greatly, at the bottom of production efficiency, operate complicated, three waste discharge large, poor product quality, the content of the vinyl isobutyl ether obtained is about 92%.
Summary of the invention
Instant invention overcomes the defect of prior art, the method for purification of the vinyl isobutyl ether that a kind of good product quality, production efficiency are high, three waste discharge is few is provided.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: a kind of method of purification of vinyl isobutyl ether, comprises the following steps:
(1) be that the vinyl isobutyl ether solution of 50-90% carries out rectification under vacuum by mass percentage concentration, obtaining take vinyl isobutyl ether as the distillate of main component, take isopropylcarbinol as the kettle base solution of main component, rectification temperature is 50 ~ 95 DEG C, and pressure is 10 ~ 60kPa;
(2) the distillate deionized water of above-mentioned steps (1) is carried out wash, layering, obtain upper strata organism phase and lower floor's aqueous phase, be separated organic phase and namely obtain the vinyl isobutyl ether that mass percentage concentration is 97% ~ 99.5%.
Further:
The mass percentage concentration of the vinyl isobutyl ether solution in the present invention described in step (1) is 60-90%.
Rectification temperature in the present invention described in step (1) is 65 ~ 85 DEG C, and pressure is 20 ~ 50kPa.
In the present invention, the mass ratio of step (2) described deionized water and distillate medium vinyl isobutyl ether is 1:2 ~ 6, is preferably 1:3 ~ 5; Wash temperature is 5 ~ 20 DEG C, is preferably 10 ~ 15 DEG C.
Lower floor's aqueous phase described in above-mentioned steps (2) can be carried out atmospheric distillation in the present invention, obtain overhead fraction and tower bottoms, rectification temperature is 90-120 DEG C, utilized by the feedstock circulation of described overhead fraction as the catalyzer preparing synthesis of vinyl isobutyl ether, tower bottoms utilizes as the feeding cycle of deionized water wash.
Under the present invention utilizes different pressures, alcohol ether azeotropic forms different principles, rectification under vacuum is carried out to the vinyl isobutyl ether solution that mass percentage concentration is 50-90%, the purity of vinyl isobutyl ether is increased to about 97%, again with deionized water carry out washing, layering, isopropylcarbinol in removing distillate, finally obtains the vinyl isobutyl ether of 97% ~ 99.5%.
The temperature of rectification under vacuum is the principal element affecting rectification effect, and temperature is too low, and the purity obtaining product can be made not reach required index, temperature is too high, can make product variable color, affect final product quality, therefore in the present invention, rectification temperature is 50 ~ 95 DEG C, preferably 65 ~ 85 DEG C.
Pressure is also very large to the influential effect of rectification under vacuum, and pressure is too low, product vapor condensation difficulty, and energy consumption is large, pressure is too high, and product rectification temperature is too high, affects finished product colourity, thus affecting final product quality, the pressure of therefore rectification under vacuum in the present invention is 10 ~ 60kPa, preferably 20 ~ 50kPa.
When washing with the distillate of deionized water to rectification under vacuum, the mass ratio of deionized water and distillate medium vinyl isobutyl ether is the principal element affecting washing effect.During washing, deionized water consumption is larger, and washing effect is better, and after washing, in product, isopropylcarbinol content is lower; But deionized water consumption is too large, material consumption increases, uneconomical, and when deionized water is increased to certain limit, washing effect increases not obvious.Therefore in the present invention, the mass ratio of deionized water and distillate medium vinyl isobutyl ether is 1:2 ~ 6, is preferably 1:3 ~ 5.
Temperature when washing with the distillate of deionized water on rectification under vacuum also has impact to washing effect, and temperature is too high, and product vaporization is serious, energy consumption increases, and temperature is too low, and washing effect is poor, washing time is long, and therefore in the present invention, wash temperature is 5 ~ 20 DEG C, is preferably 10 ~ 15 DEG C.
In the present invention, the kettle base solution that rectification under vacuum obtains is the isopropylcarbinol that mass percentage concentration is greater than 98.5%, and the feedstock circulation of the recyclable catalyzer as preparing synthesis of vinyl isobutyl ether utilizes; In addition, the lower floor's aqueous phase obtained after washing, layering can be carried out atmospheric distillation, after the overhead fractions such as the isopropylcarbinol be separated, a small amount of vinyl isobutyl ether are recyclable, feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes, and tower bottoms reduces production cost further as the feeding cycle utilization of washing.
The present invention compared with prior art has the following advantages:
1, decrease the consumption of deionized water during washing, saved washing time, improve production efficiency, reduced production cost;
2, material reusable edible, decreases three waste discharge, improves environmental benefit;
3, good product quality, after purifying, vinyl isobutyl ether content is more than 98.5%;
Method of the present invention also can adopt full-automatic DCS Long-distance Control on production equipment, saves labor force, enhances productivity further.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
As shown in the figure: 1 is synthetic tower, 2 is the first rectifying tower, and 3 for reclaiming alcohol storage tank, and 4 is water wash column, and 5 is pan tank, and 6 is alcohol water collecting groove, and 7 is Second distillation column, and 8 is recovery system
Embodiment
Below by way of drawings and Examples, the present invention is described in further details, but the present invention is not limited to described embodiment.
Embodiment 1
Is that the solution of the vinyl isobutyl ether of 90% squeezes into the first rectifying tower 2 by synthetic tower 1 containing mass percentage concentration, pressure be 20kPa, under bottom temperature is the condition of 65 DEG C, carry out rectification under vacuum, the kettle base solution that rectification under vacuum obtains is the isopropylcarbinol that mass percentage concentration is greater than 98.5%, squeezed into and reclaim alcohol storage tank 3, the feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes; Overhead distillate is the vinyl isobutyl ether that mass percentage concentration is greater than 97%, entered water wash column 4 deionized water circulation cleaning, isopropylcarbinol in removing distillate, during washing, the mass ratio of deionized water and distillate medium vinyl isobutyl ether controls at 1:3, and washing temperature is 10 DEG C; The material static layering obtained by water wash column 4, obtains upper organic phase and lower floor's inorganic phase, and be separated organic phase and namely obtain finished product vinyl isobutyl ether, sampling analysis product content is 99.5%, is sent into pan tank 5; Lower floor's inorganic phase enters Second distillation column 7 after alcohol water collecting groove 6 is collected, rectifying is carried out under being the condition of 100 DEG C in normal pressure, temperature, the isopropylcarbinol be separated, a small amount of vinyl isobutyl ether enter recovery system 8 as overhead fraction, feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes, and tower bottoms utilizes as the feeding cycle of water wash column 4.
Embodiment 2
Is that the solution of the vinyl isobutyl ether of 75% squeezes into the first rectifying tower 2 by synthetic tower 1 containing mass percentage concentration, pressure be 25kPa, under bottom temperature is the condition of 70 DEG C, carry out rectification under vacuum, the kettle base solution that rectification under vacuum obtains is the isopropylcarbinol that mass percentage concentration is greater than 98.5%, squeezed into and reclaim alcohol storage tank 3, the feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes; Overhead distillate is the vinyl isobutyl ether that mass percentage concentration is greater than 97%, entered water wash column 4 deionized water circulation cleaning, isopropylcarbinol in removing distillate, during washing, the mass ratio of deionized water and distillate medium vinyl isobutyl ether controls at 1:4, and washing temperature is 13 DEG C; The material static layering obtained by water wash column 4, obtains upper organic phase and lower floor's inorganic phase, and be separated organic phase and namely obtain finished product vinyl isobutyl ether, sampling analysis product content is 99%, is sent into pan tank 5; Lower floor's inorganic phase enters Second distillation column 7 after alcohol water collecting groove 6 is collected, rectifying is carried out under being the condition of 104 DEG C in normal pressure, temperature, the isopropylcarbinol be separated, a small amount of vinyl isobutyl ether enter recovery system 8 as overhead fraction, feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes, and tower bottoms utilizes as the feeding cycle of water wash column 4.
Embodiment 3
Is that the solution of the vinyl isobutyl ether of 65% squeezes into the first rectifying tower 2 by synthetic tower 1 containing mass percentage concentration, pressure be 45kPa, under bottom temperature is the condition of 80 DEG C, carry out rectification under vacuum, the kettle base solution that rectification under vacuum obtains is the isopropylcarbinol that mass percentage concentration is greater than 98.5%, squeezed into and reclaim alcohol storage tank 3, the feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes; Overhead distillate is the vinyl isobutyl ether that mass percentage concentration is greater than 97%, entered water wash column 4 deionized water circulation cleaning, isopropylcarbinol in removing distillate, during washing, the mass ratio of deionized water and distillate medium vinyl isobutyl ether controls at 1:5, and washing temperature is 15 DEG C; The material static layering obtained by water wash column 4, obtains upper organic phase and lower floor's inorganic phase, and be separated organic phase and namely obtain finished product vinyl isobutyl ether, sampling analysis product content is 99%, is sent into pan tank 5; Lower floor's inorganic phase enters Second distillation column 7 after alcohol water collecting groove 6 is collected, rectifying is carried out under being the condition of 108 DEG C in normal pressure, temperature, the isopropylcarbinol be separated, a small amount of vinyl isobutyl ether enter recovery system 8 as overhead fraction, feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes, and tower bottoms utilizes as the feeding cycle of water wash column 4.
Embodiment 4
Is that the solution of the vinyl isobutyl ether of 60% squeezes into the first rectifying tower 2 by synthetic tower 1 containing mass percentage concentration, pressure be 50kPa, under bottom temperature is the condition of 85 DEG C, carry out rectification under vacuum, the kettle base solution that rectification under vacuum obtains is the isopropylcarbinol that mass percentage concentration is greater than 98.5%, squeezed into and reclaim alcohol storage tank 3, the feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes; Overhead distillate is the vinyl isobutyl ether that mass percentage concentration is greater than 97%, entered water wash column 4 deionized water circulation cleaning, isopropylcarbinol in removing distillate, during washing, the mass ratio of deionized water and distillate medium vinyl isobutyl ether controls at 1:5, and washing temperature is 18 DEG C; The material static layering obtained by water wash column 4, obtains upper organic phase and lower floor's inorganic phase, and be separated organic phase and namely obtain finished product vinyl isobutyl ether, sampling analysis product content is 98.5%, is sent into pan tank 5; Lower floor's inorganic phase enters Second distillation column 7 after alcohol water collecting groove 6 is collected, rectifying is carried out under being the condition of 105 DEG C in normal pressure, temperature, the isopropylcarbinol be separated, a small amount of vinyl isobutyl ether enter recovery system 8 as overhead fraction, feedstock circulation as the catalyzer preparing synthesis of vinyl isobutyl ether utilizes, and tower bottoms utilizes as the feeding cycle of water wash column 4.
Claims (1)
1. a method of purification for vinyl isobutyl ether, is characterized in that, comprises the following steps:
(1) be that the vinyl isobutyl ether solution of 60-90% carries out rectification under vacuum by mass percentage concentration, obtain with vinyl isobutyl ether be main component distillate and take isopropylcarbinol as the kettle base solution of main component, rectification temperature is 65 ~ 85 DEG C, and pressure is 20 ~ 50kPa;
(2) the distillate deionized water of above-mentioned steps (1) is washed, layering, obtain upper strata organism phase and lower floor's aqueous phase, the mass ratio of described deionized water and distillate medium vinyl isobutyl ether is 1:3 ~ 5, wash temperature is 10 ~ 15 DEG C, be separated organic phase and namely obtain the vinyl isobutyl ether that mass percentage concentration is 98.5% ~ 99.5%, simultaneously, described lower floor's aqueous phase is carried out atmospheric distillation, obtain overhead fraction and tower bottoms, rectification temperature is 90-120 DEG C, the feedstock circulation of described overhead fraction as the catalyzer preparing synthesis of vinyl isobutyl ether is utilized, tower bottoms utilizes as the feeding cycle of deionized water wash.
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| CN201210176295.9A CN102701920B (en) | 2012-05-29 | 2012-05-29 | Method for purifying vinyl isobutyl ether |
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| CN201210176295.9A CN102701920B (en) | 2012-05-29 | 2012-05-29 | Method for purifying vinyl isobutyl ether |
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| CN102701920B true CN102701920B (en) | 2015-03-18 |
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| CN106986888B (en) * | 2017-04-03 | 2019-01-01 | 江苏艾科维科技有限公司 | The discoloration method of ketoxime type silane crosslinker |
| CN106977360B (en) * | 2017-04-18 | 2019-10-11 | 山东赛托生物科技股份有限公司 | A method of toluene and diethoxymethane are recycled from 17 Alpha-hydroxy progesterone production waste liquid |
| CN113200828B (en) * | 2021-05-04 | 2022-04-26 | 浙江锦华新材料股份有限公司 | Refining method of vinyl isobutyl ether |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401619A (en) * | 2002-09-17 | 2003-03-12 | 刘琳 | Method and apparatus for continuous synthesis of vinyl isobutyl ether |
| WO2004096741A2 (en) * | 2003-04-30 | 2004-11-11 | Basf Aktiengesellschaft | Continuous method for producing methyl vinyl ether |
| CN1709847A (en) * | 2005-06-21 | 2005-12-21 | 孟永华 | Continuous synthesizing method of vinyl isobutyl ether |
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- 2012-05-29 CN CN201210176295.9A patent/CN102701920B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401619A (en) * | 2002-09-17 | 2003-03-12 | 刘琳 | Method and apparatus for continuous synthesis of vinyl isobutyl ether |
| WO2004096741A2 (en) * | 2003-04-30 | 2004-11-11 | Basf Aktiengesellschaft | Continuous method for producing methyl vinyl ether |
| CN1709847A (en) * | 2005-06-21 | 2005-12-21 | 孟永华 | Continuous synthesizing method of vinyl isobutyl ether |
Non-Patent Citations (2)
| Title |
|---|
| 异丁基乙烯基醚的合成;林军;《浙江化工》;20061231;第37卷(第12期);第1-3页 * |
| 羟丁基乙烯基醚的合成;汪伟志等;《化学世界》;20021231(第10期);第540-543页 * |
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