CN102976904B - Preparation device of isobutyl vinyl ether and preparation method thereof - Google Patents
Preparation device of isobutyl vinyl ether and preparation method thereof Download PDFInfo
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- CN102976904B CN102976904B CN201210570442.0A CN201210570442A CN102976904B CN 102976904 B CN102976904 B CN 102976904B CN 201210570442 A CN201210570442 A CN 201210570442A CN 102976904 B CN102976904 B CN 102976904B
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- ive
- tubular reactor
- isopropylcarbinol
- vinyl ether
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Abstract
The invention discloses a preparation device of isobutyl vinyl ether and a preparation method of isobutyl vinyl ether, which relates to isobutyl vinyl ether. The invention provides the preparation device of isobutyl vinyl ether and the preparation method of isobutyl vinyl ether. The preparation device of isobutyl vinyl ether is safe, efficient, low in energy consumption, low in cost and easy to industrialize. The device is provided with an absorber, a gas-liquid separator, a metering pump, a constant temperature oil bath, a tubular reactor, a condenser and a reducing valve. The preparation method comprises the following steps: 1) dissolving acetylene in a saturated solution formed by isobutanol and catalyst solutions; 2) pressurizing the saturated solution obtained in step 1) to 1-5MPa by the metering pump and introducing the saturated solution to the heated tubular reactor, wherein acetylene dissolved in the isobutanol and catalyst solutions react with isobutanol in the tubular reactor to generate isobutyl vinyl ether; and 3) cooling reactants sent from the tubular reactor, wherein part of the reactants is used as a coarse product of isobutyl vinyl ether and the rest of the reactants is circulated to step 1) and mixed with continuously fed isobutanol and catalyst solutions.
Description
Technical field
The present invention relates to IVE, especially relate to a kind of IVE preparation facilities and preparation method thereof.
Background technology
IVE is important organic synthesis intermediate and the monomer of polymkeric substance.The polymkeric substance that the IVE of take is main raw material is widely used in the fields such as coating, tackiness agent and ink.
IVE adopts acetylene and isopropylcarbinol synthetic under certain pressure and temperature conventionally.One class preparation method is that reaction unit adopts high pressure tank reactor (referring to document: < < Zhejiang chemical industry > >, 2006,12:1-3; Chinese patent 200810062915.X).The method need to be take a large amount of xylidines as solvent, and catalyst levels very large (be isopropylcarbinol weight 8～20%), causes cost very high.High pressure tank reactor can only periodical operation, and depresses for the reaction that acetylene participates in for adding, and is difficult to safe amplification, thereby can only prepares on a small quantity for laboratory, is difficult to industrialization.
The another kind of method of preparing IVE is to adopt the withstand voltage tower reactor of operate continuously (referring to Chinese patent 02138285.9; Chinese patent 200510040652.9).The gas mixture of acetylene and nitrogen, after compressor pressurization, passes into from tower reactor bottom, and the isopropylcarbinol under with tower top top spray reacts with reverse contact of catalyzer.This method reactor manufacturing cost is high, has certain danger, and safe reliability is poor.In reactor, gas-liquid mass transfer efficiency is low, and catalyst levels is very large.A large amount of unreacted acetylene and nitrogen circulation make the energy consumption of compressor very large.
Summary of the invention
The object of the present invention is to provide a kind of safe, efficient, less energy-consumption, low cost and be easy to industrialized a kind of IVE preparation facilities and preparation method thereof.
Described IVE preparation facilities is provided with resorber, gas-liquid separator, volume pump, thermostatical oil bath, tubular reactor, condenser and reducing valve; The material outlet of described absorber bottom connects the material inlet of gas-liquid separator, and the material outlet of gas-liquid separator is through the material inlet of volume pump take-over type reactor; Described tubular reactor is placed in thermostatical oil bath to keep certain temperature of reaction; The outlet of described tubular reactor connects the material inlet of condenser, and the material outlet of condenser connects the material inlet of reducing valve, and the material outlet of reducing valve connects respectively liquid material entrance and the outlet for product of resorber.
Described resorber can adopt stirring tank.
Described tubular reactor can adopt stainless steel tube.
The preparation method of described IVE, comprises the following steps:
1) acetylene is dissolved in isopropylcarbinol and catalyst solution and forms saturated solution;
In step 1), describedly acetylene is dissolved in to condition in isopropylcarbinol and catalyst solution can under 5～40 ℃ and normal pressure, carries out; Described catalyzer can be selected from isopropylcarbinol potassium etc.; The consumption of catalyzer can be 1%～3% of isopropylcarbinol quality.
2) saturated solution with volume pump, step 1) being obtained is forced into 1～5MPa and passes in the tubular reactor having heated, and the acetylene and the isopropylcarbinol that are dissolved in isopropylcarbinol and catalyst solution react in tubular reactor, generates IVE;
In step 2) in, the temperature of described heating can be 120～170 ℃; The temperature of described reaction can be 120～170 ℃, and the pressure of reaction can be 1～5MPa.
3) the cooling reaction product of sending from tubular reactor, partial reaction product is as the thick product of IVE, and rest part loops back step 1) and mixes with isopropylcarbinol and the catalyst solution of continuously feeding.
In the thick product of IVE, through extracting rectifying, to make purity be more than 99% IVE product for IVE and unreacted isopropylcarbinol.The recycle of unreacted isopropylcarbinol.The total recovery of IVE reaches more than 96%.
Compare with the technique of existing preparation IVE, tool of the present invention has the following advantages:
1) in reactor, reaction system is liquid phase, does not have acetylene in gas phase, thereby has avoided the danger of gas phase acetylene blast under High Temperature High Pressure;
2) reaction system is homogeneous phase, not limited by gas-liquid mass transfer, has improved speed of reaction and transformation efficiency.
3) tubular reactor adopting is a stainless steel tube, and simple in structure, volume is little, and cost is low, can adopt simply shell and tube to be amplified to technical scale, has avoided scale effect.
4) reactor heat transfer characteristic is fabulous, and inside reactor temperature is even.
5) do not use acetylene compressor, gas does not circulate, and energy consumption reduces greatly.
6) catalyst levels reduces greatly.
Accompanying drawing explanation
Fig. 1 is process unit schematic diagram of the present invention.In Fig. 1, be respectively labeled as: the 1st, resorber, the 2nd, gas-liquid separator, the 3rd, volume pump, the 4th, thermostatical oil bath, the 5th, tubular reactor, the 6th, condenser, the 7th, reducing valve.
Embodiment
The invention will be further described in connection with accompanying drawing for following examples:
Embodiment 1:
The reaction of acetylene and isopropylcarbinol adopts the circulating reaction device being comprised of resorber 1, gas-liquid separator 2, volume pump 3, thermostatical oil bath 4, tubular reactor 5, condenser 6 and reducing valve 7 etc. shown in Fig. 1.Tubular reactor 5 is internal diameter 2mm, the stainless steel tube of length 32m, and reactor volume is about 100ml.Process conditions is as follows:
Catalyst levels: be 1.5% of isopropylcarbinol total mass;
Feed rate: 200g/h;
Absorber temperatures: 25 ℃;
Absorber pressure: 0.105MPa;
Temperature of reactor: 150 ℃;
Reactor pressure: 4MPa;
Cycle rate: 3.6L/h.
Through about 3h operation, circulating reaction system reaches stable state.Reaction product discharging speed 241g/h, isopropylcarbinol transformation efficiency is 65%, reaction is 98.6% to the selectivity of IVE.
Embodiment 2:
The reaction of acetylene and isopropylcarbinol adopts the circulating reaction device shown in Fig. 1.Tubular reactor is internal diameter 2mm, the stainless steel tube of length 32m.Reactor volume is about 100ml.Process conditions is as follows:
Catalyst levels: be 2% of isopropylcarbinol total mass;
Feed rate: 200g/h;
Absorber temperatures: 25 ℃;
Absorber pressure: 0.105MPa;
Temperature of reactor: 160 ℃;
Reactor pressure: 4MPa;
Cycle rate: 3.6L/h.
Through 3h operation, circulating reaction system reaches stable state.Reaction product discharging speed 248g/h, isopropylcarbinol transformation efficiency is 75%, reaction is 96.5% to the selectivity of IVE.
Embodiment 3:
The reaction of acetylene and isopropylcarbinol adopts the circulating reaction device shown in Fig. 1.Tubular reactor is internal diameter 2mm, the stainless steel tube of length 32m, and reactor volume is about 100ml.Process conditions is as follows:
Catalyst content: be 1% of isopropylcarbinol total mass;
Feed rate: 200g/h;
Absorber temperatures: 15 ℃;
Absorber pressure: 0.105MPa;
Temperature of reactor: 140 ℃;
Reactor pressure: 3MPa;
Cycle rate: 3.6L/h.
Through 3h operation, circulating reaction system reaches stable state.Reaction product discharging speed 231g/h, isopropylcarbinol transformation efficiency is 55%, reaction is 99% to the selectivity of IVE.
Claims (7)
1. an IVE preparation facilities, is characterized in that being provided with resorber, gas-liquid separator, volume pump, thermostatical oil bath, tubular reactor, condenser and reducing valve; The material outlet of described absorber bottom connects the material inlet of gas-liquid separator, and the material outlet of gas-liquid separator is through the material inlet of volume pump take-over type reactor; Described tubular reactor is placed in thermostatical oil bath to keep certain temperature of reaction; The outlet of described tubular reactor connects the material inlet of condenser, and the material outlet of condenser connects the material inlet of reducing valve, and the material outlet of reducing valve connects respectively liquid material entrance and the outlet for product of resorber.
2. a kind of IVE preparation facilities as claimed in claim 1, is characterized in that described resorber adopts stirring tank.
3. a kind of IVE preparation facilities as claimed in claim 1, is characterized in that described tubular reactor adopts stainless steel tube.
4. a preparation method for IVE, is characterized in that adopting IVE preparation facilities as claimed in claim 1, and described preparation method comprises the following steps:
1) acetylene is dissolved in isopropylcarbinol and catalyst solution and forms saturated solution; Describedly acetylene is dissolved in to condition in isopropylcarbinol and catalyst solution under 5～40 ℃ and normal pressure, carries out; The consumption of described catalyzer is 1%～3% of isopropylcarbinol quality;
2) with volume pump by step 1) saturated solution that obtains is forced into 1～5MPa and passes in the tubular reactor having heated, the acetylene and the isopropylcarbinol that are dissolved in isopropylcarbinol and catalyst solution react in tubular reactor, generate IVE;
3) the cooling reaction product of sending from tubular reactor, partial reaction product is as the thick product of IVE, rest part loops back step 1) and mix with isopropylcarbinol and the catalyst solution of continuously feeding.
5. a kind of preparation method of IVE as claimed in claim 4, is characterized in that in step 1) in, described catalyzer is selected from isobutyl potassium alcoholate.
6. a kind of preparation method of IVE as claimed in claim 4, is characterized in that in step 2) in, the temperature of described heating is 120～170 ℃.
7. a kind of preparation method of IVE as claimed in claim 4, is characterized in that in step 2) in, the temperature of described reaction is 120～170 ℃, the pressure of reaction is 1～5MPa.
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| CN201210570442.0A CN102976904B (en) | 2012-12-24 | 2012-12-24 | Preparation device of isobutyl vinyl ether and preparation method thereof |
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| CN201210570442.0A CN102976904B (en) | 2012-12-24 | 2012-12-24 | Preparation device of isobutyl vinyl ether and preparation method thereof |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103382090B (en) * | 2013-07-11 | 2015-10-28 | 徐东 | A kind of method of continuous production copper-zinc-tin-sulfur film |
| CN105837407A (en) * | 2016-04-27 | 2016-08-10 | 厦门大学 | Preparation method of isobutyl vinyl ether |
| CN111875481A (en) * | 2020-08-21 | 2020-11-03 | 菏泽华立新材料有限公司 | Continuous production process and equipment for dihydric alcohol vinyl ether |
| CN116724017A (en) * | 2021-02-04 | 2023-09-08 | 丸善石油化学株式会社 | Method for producing isobutyl vinyl ether and method for purifying isobutyl vinyl ether |
| 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 |
| CN115490575A (en) * | 2022-10-13 | 2022-12-20 | 辽宁惠风生物医药科技有限公司 | Preparation method of 2-ethoxypropylene |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB683682A (en) * | 1944-07-04 | 1952-12-03 | Montedison Spa | Improvements in and relating to processes for the production of vinylic ethers |
| US5726321A (en) * | 1995-03-24 | 1998-03-10 | Basf Aktiengesellschaft | Process for carrying out gas/liquid reactions under avoidance of a continuous gas phase |
| CN1444552A (en) * | 2000-04-06 | 2003-09-24 | 巴斯福股份公司 | Method for producing alkenyl ethers |
| CN1780804A (en) * | 2003-04-30 | 2006-05-31 | 巴斯福股份公司 | Continuous method for producing methyl vinyl ether |
| CN101898939A (en) * | 2010-08-06 | 2010-12-01 | 湖北新景新材料有限公司 | Method for preparing compound 4-hydroxy butyl vinyl ether |
-
2012
- 2012-12-24 CN CN201210570442.0A patent/CN102976904B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB683682A (en) * | 1944-07-04 | 1952-12-03 | Montedison Spa | Improvements in and relating to processes for the production of vinylic ethers |
| US5726321A (en) * | 1995-03-24 | 1998-03-10 | Basf Aktiengesellschaft | Process for carrying out gas/liquid reactions under avoidance of a continuous gas phase |
| CN1444552A (en) * | 2000-04-06 | 2003-09-24 | 巴斯福股份公司 | Method for producing alkenyl ethers |
| CN1780804A (en) * | 2003-04-30 | 2006-05-31 | 巴斯福股份公司 | Continuous method for producing methyl vinyl ether |
| CN101898939A (en) * | 2010-08-06 | 2010-12-01 | 湖北新景新材料有限公司 | Method for preparing compound 4-hydroxy butyl vinyl ether |
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