CN1709847A - Continuous synthesizing method of vinyl isobutyl ether - Google Patents
Continuous synthesizing method of vinyl isobutyl ether Download PDFInfo
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- CN1709847A CN1709847A CN 200510040652 CN200510040652A CN1709847A CN 1709847 A CN1709847 A CN 1709847A CN 200510040652 CN200510040652 CN 200510040652 CN 200510040652 A CN200510040652 A CN 200510040652A CN 1709847 A CN1709847 A CN 1709847A
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- acetylene
- isobutyl ether
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Abstract
This invention has disclosed a kind of continuous sythesizing method for vinyl-isobutyl ether. It regards acetylene and isobutyl alcohol as reaction raw materials, process synthesis reaction in converter, within which fills the catalyst solution with liquid location 50-80 percent. Acetylene and isobutyl alcohol gas get into the tower from converter bottom muzzle after mixed evenly, catalyst solution in the bottom get to top of the tower successively through circulation pump, carrying on circulation, after the small acetylene air bubble meet the isobutyl alcohol, they take etherification in converter, the etherification temperature is 125-150Deg. C, the converter pressure is 0.3-0.6Mpa; the catalyst is isobutyl alcohol solution including KOH, vinyl-isobutyl ether produced in reaction and acetylene and isobutyl alcohol not reacting, export from the top of the converter, through condenser it enter receive pot, then can make the vinyl-isobutyl ether of the finished product by the after-treatment. This reaction is safe and its reliability is good, the one way conversion ratio of acetylene and synthesis reaction harvest rate are high, the content of acetylene is low in the tail gas.
Description
Technical field:
The present invention relates to a kind of method for continuously synthesizing of vinyl isobutyl ether.Belong to technical field of organic synthesis.
Background technology:
Vinyl isobutyl ether is the main raw material of polymerizing vinyl chloride-vinyl isobutyl ether, also is that medicine is synthetic, the intermediate of Chemical Manufacture.Before the present invention makes, adopt acetylene to carry out the continuous synthesis of vinyl isobutyl ether of etherification reaction (CN021382589) with isopropylcarbinol reverse contact in synthetic tower usually with nitrogen mixture.There is certain danger in this method, and security is reliably relatively poor.Acetylene per pass conversion and building-up reactions yield are low, and the purity of reaction product vinyl isobutyl ether is low, the acetylene content height of exhaust emissions: the acetylene per pass conversion is more than 75%, and the building-up reactions yield is (in acetylene) more than 95%.The acetylene content of exhaust emissions is below 0.5%.
Summary of the invention:
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of reaction safe reliability good, acetylene per pass conversion and building-up reactions yield height, the method for continuously synthesizing of the purity height of reaction product vinyl isobutyl ether, vinyl isobutyl ether that the acetylene content of exhaust emissions is low.
The object of the present invention is achieved like this: a kind of method for continuously synthesizing of vinyl isobutyl ether, it is characterized in that it is is reaction raw materials with acetylene and isopropylcarbinol, in synthetic tower, carry out building-up reactions, be filled with the catalyst solution of 50～80% liquid levels in the synthetic tower, described acetylene and isobutanol gas, at the bottom of synthetic tower, after mixing, nozzle feeds synthetic tower, catalyst solution at the bottom of the tower is continuously got to cat head by recycle pump, circulate, the acetylene small bubbles that form with synthesize etherification reaction after isopropylcarbinol contacts in synthetic tower, the temperature of etherification reaction is: 125～150 ℃, reaction pressure 0.3～the 0.6Mpa of synthetic tower, catalyzer is the isobutanol solution that contains KOH, vinyl isobutyl ether and unreacted acetylene that reaction generates, isopropylcarbinol is derived by the synthetic tower cat head, behind condenser, enter receiving tank, can make the finished product vinyl isobutyl ether through aftertreatment again.
The method for continuously synthesizing of vinyl isobutyl ether of the present invention, described catalyzer contain that KOH content is 12～20% in the isobutanol solution of KOH.
Compare with the method for existing continuous synthesis of vinyl isobutyl ether, the present invention has following advantage:
The present invention is before acetylene enters synthetic tower; mix by nozzle with isobutanol gas earlier; isopropylcarbinol plays a protective role to acetylene gas; greatly reduce acetylene and give birth to dangerous possibility in high temperature, elevated pressure; and acetylene per pass conversion and reaction yield have been improved; improve the purity of reaction product vinyl isobutyl ether, reduced the acetylene content of exhaust emissions.React very steady, produce and be easy to control, easy and simple to handle, unit consumption is low, and production environment is clean.The present invention can make the acetylene per pass conversion reach more than 80%, and the building-up reactions yield is at (in acetylene) more than 98%, and the purity of reaction product vinyl isobutyl ether reaches more than 99.5%.The acetylene content of exhaust emissions is below 0.2%.
Description of drawings:
Fig. 1 is technological process of production figure of the present invention.
Embodiment:
Continuous synthesis of vinyl isobutyl ether:
The catalyzer that is filled with 50～80% liquid levels in the synthetic tower contains the isobutanol solution of KOH, and KOH content is 12～20% in the solution.
Behind lyophilization, enter the one-level inlet of acetylene compressor from the acetylene gas of Acetylene Gas Holder; gas enters drying tower and removes impurity after compression; subsequently; acetylene and isopropylcarbinol shielding gas; enter synthetic tower after nozzle mixes at the bottom of synthetic tower, carry out building-up reactions in synthetic tower, the recycle pump of catalyst solution at the bottom of by tower successively got to synthetic tower top; circulate, the acetylene small bubbles of formation with synthesize etherification reaction after isopropylcarbinol fully contacts in synthetic tower.The temperature of etherification reaction is controlled at 125～150 ℃, and the reaction pressure of synthetic tower is controlled at 0.3～0.6Mpa.The heat that reaction produces is taken away by the interchanger on the circulation line.Vinyl isobutyl ether that reaction generates and unreacted acetylene gas, isopropylcarbinol are derived by the synthetic tower cat head, enter receiving tank after the twice condenser condenses, can make the finished product vinyl isobutyl ether through aftertreatment again.The inlet that the unreacted acetylene gas overwhelming majority is got back to compressor directly enters synthetic tower and recycles, and seldom a part reclaims most acetylene gass wherein to the acetylene recovery system.The acetylene gas that is recovered to goes the acetylene compressor inlet to use again.
When the present invention feeds acetylene gas to synthetic tower, constantly mend into fresh catalyst solution by pump, and regularly discharge the catalyzer of inactivation to synthetic tower.
Acetylene per pass conversion 82%, the building-up reactions yield is at 98.5 (in acetylene).The acetylene content 0.19 of exhaust emissions.
The norm quota of consumption of main raw material (vinyl isobutyl ether per ton):
Acetylene: 300kg, isopropylcarbinol 800kg, catalyzer KOH80kg.
Claims (3)
1, a kind of method for continuously synthesizing of vinyl isobutyl ether, it is characterized in that it is is reaction raw materials with acetylene and isopropylcarbinol, in synthetic tower, carry out building-up reactions, be filled with the catalyst solution of 50～80% liquid levels in the synthetic tower, described acetylene and isobutanol gas, at the bottom of synthetic tower, after mixing, nozzle feeds synthetic tower, catalyst solution at the bottom of the tower is continuously got to cat head by recycle pump, circulate, the acetylene small bubbles that form with synthesize etherification reaction after isopropylcarbinol contacts in synthetic tower, the temperature of etherification reaction is: 125～150 ℃, reaction pressure 0.3～the 0.6Mpa of synthetic tower, catalyzer is the isobutanol solution that contains KOH, vinyl isobutyl ether and unreacted acetylene that reaction generates, isopropylcarbinol is derived by the synthetic tower cat head, behind condenser, enter receiving tank, can make the finished product vinyl isobutyl ether through aftertreatment again.
2, the method for continuously synthesizing of a kind of vinyl isobutyl ether according to claim 1 is characterized in that: the isobutanol solution KOH content that catalyzer contains KOH is 12～20%.
3, the method for continuously synthesizing of a kind of vinyl isobutyl ether according to claim 1 and 2, it is characterized in that: through the unreacted acetylene gas of synthetic tower, the inlet that the overwhelming majority is got back to compressor directly enters synthetic tower and recycles, seldom a part is to the acetylene recovery system, reclaim and use, the acetylene gas that is recovered to goes the acetylene compressor inlet to use again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510040652 CN1709847A (en) | 2005-06-21 | 2005-06-21 | Continuous synthesizing method of vinyl isobutyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510040652 CN1709847A (en) | 2005-06-21 | 2005-06-21 | Continuous synthesizing method of vinyl isobutyl ether |
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| Publication Number | Publication Date |
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| CN1709847A true CN1709847A (en) | 2005-12-21 |
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Family Applications (1)
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| CN 200510040652 Pending CN1709847A (en) | 2005-06-21 | 2005-06-21 | Continuous synthesizing method of vinyl isobutyl ether |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701920A (en) * | 2012-05-29 | 2012-10-03 | 浙江锦华新材料股份有限公司 | Method for purifying vinyl isobutyl ether |
| CN101555198B (en) * | 2008-07-10 | 2014-01-15 | 杭州电化集团有限公司 | Synthesis method of isobutyl vinyl ether and device thereof |
| CN113173837A (en) * | 2021-04-24 | 2021-07-27 | 浙江锦华新材料股份有限公司 | Preparation method of vinyl isobutyl ether |
| CN113200828A (en) * | 2021-05-04 | 2021-08-03 | 浙江锦华新材料股份有限公司 | Refining method of vinyl isobutyl ether |
| CN115490575A (en) * | 2022-10-13 | 2022-12-20 | 辽宁惠风生物医药科技有限公司 | A kind of preparation method of 2-ethoxypropene |
| CN115974657A (en) * | 2022-12-06 | 2023-04-18 | 浙江皇马科技股份有限公司 | Process method and system for preparing vinyl ether by reaction of high-boiling-point monohydric alcohol and acetylene |
-
2005
- 2005-06-21 CN CN 200510040652 patent/CN1709847A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555198B (en) * | 2008-07-10 | 2014-01-15 | 杭州电化集团有限公司 | Synthesis method of isobutyl vinyl ether and device thereof |
| CN102701920A (en) * | 2012-05-29 | 2012-10-03 | 浙江锦华新材料股份有限公司 | Method for purifying vinyl isobutyl ether |
| CN102701920B (en) * | 2012-05-29 | 2015-03-18 | 浙江锦华新材料股份有限公司 | Method for purifying vinyl isobutyl ether |
| CN113173837A (en) * | 2021-04-24 | 2021-07-27 | 浙江锦华新材料股份有限公司 | Preparation method of vinyl isobutyl ether |
| CN113173837B (en) * | 2021-04-24 | 2022-05-06 | 浙江锦华新材料股份有限公司 | Preparation method of vinyl isobutyl ether |
| CN113200828A (en) * | 2021-05-04 | 2021-08-03 | 浙江锦华新材料股份有限公司 | Refining method of vinyl isobutyl ether |
| CN115490575A (en) * | 2022-10-13 | 2022-12-20 | 辽宁惠风生物医药科技有限公司 | A kind of preparation method of 2-ethoxypropene |
| CN115974657A (en) * | 2022-12-06 | 2023-04-18 | 浙江皇马科技股份有限公司 | Process method and system for preparing vinyl ether by reaction of high-boiling-point monohydric alcohol and acetylene |
| CN115974657B (en) * | 2022-12-06 | 2024-10-01 | 浙江皇马科技股份有限公司 | Process method and system for preparing vinyl ether by reacting high-boiling monohydric alcohol with acetylene |
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