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Preparation device of isobutyl vinyl ether and preparation method thereof

A technology for isobutyl vinyl ether and preparation equipment, which is applied in ether preparation, ether preparation by addition of unsaturated compounds, organic chemistry, etc., and can solve the problems of high reactor manufacturing cost, low gas-liquid mass transfer efficiency, and poor safety and reliability and other problems, to achieve the effect of simple structure, avoiding amplification effect and low cost

Inactive Publication Date: 2013-03-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The manufacturing cost of the reactor in this method is high, there is a certain risk, and the safety and reliability are poor.
The gas-liquid mass transfer efficiency in the reactor is low, and the amount of catalyst is large
A large amount of unreacted acetylene and nitrogen cycle makes the energy consumption of the compressor very high

Method used

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  • Preparation device of isobutyl vinyl ether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The reaction of acetylene and isobutanol uses figure 1 The shown circulation reaction device is composed of absorber 1, gas-liquid separator 2, metering pump 3, constant temperature oil bath 4, tubular reactor 5, condenser 6 and pressure reducing valve 7, etc. The tubular reactor 5 is a stainless steel tube with an inner diameter of 2 mm and a length of 32 m, and the volume of the reactor is about 100 ml. The process operating conditions are as follows:

[0027] Catalyst dosage: 1.5% of the total mass of isobutanol;

[0028] Feed flow: 200g / h;

[0029] Absorber temperature: 25°C;

[0030] Absorber pressure: 0.105MPa;

[0031] Reactor temperature: 150°C;

[0032] Reactor pressure: 4MPa;

[0033] Circulation rate: 3.6L / h.

[0034] After about 3 hours of operation, the cyclic reaction system reached a steady state. The discharge rate of the reaction product was 241 g / h, the conversion rate of isobutanol was 65%, and the selectivity of the reaction to isobutyl vinyl...

Embodiment 2

[0036] The reaction of acetylene and isobutanol uses figure 1 The cyclic reaction apparatus shown. The tubular reactor is a stainless steel tube with an inner diameter of 2mm and a length of 32m. The reactor volume is about 100ml. The process operating conditions are as follows:

[0037] Catalyst dosage: 2% of the total mass of isobutanol;

[0038] Feed flow: 200g / h;

[0039] Absorber temperature: 25°C;

[0040] Absorber pressure: 0.105MPa;

[0041] Reactor temperature: 160°C;

[0042] Reactor pressure: 4MPa;

[0043] Circulation rate: 3.6L / h.

[0044] After 3 hours of operation, the cyclic reaction system reached a steady state. The discharge rate of the reaction product was 248g / h, the conversion rate of isobutanol was 75%, and the selectivity of the reaction to isobutyl vinyl ether was 96.5%.

Embodiment 3

[0046] The reaction of acetylene and isobutanol uses figure 1 The cyclic reaction apparatus shown. The tubular reactor is a stainless steel tube with an inner diameter of 2mm and a length of 32m, and the volume of the reactor is about 100ml. The process operating conditions are as follows:

[0047] Catalyst content: 1% of the total mass of isobutanol;

[0048] Feed flow: 200g / h;

[0049] Absorber temperature: 15°C;

[0050] Absorber pressure: 0.105MPa;

[0051] Reactor temperature: 140°C;

[0052] Reactor pressure: 3MPa;

[0053] Circulation rate: 3.6L / h.

[0054] After 3 hours of operation, the cyclic reaction system reached a steady state. The discharge rate of the reaction product was 231 g / h, the conversion rate of isobutanol was 55%, and the selectivity of the reaction to isobutyl vinyl ether was 99%.

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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 [0001] The invention relates to isobutyl vinyl ether, in particular to an isobutyl vinyl ether preparation device and a preparation method thereof. Background technique [0002] Isobutyl vinyl ether is an important organic synthesis intermediate and polymer monomer. Polymers based on isobutyl vinyl ether are widely used in the fields of coatings, adhesives and inks. [0003] Isobutyl vinyl ether is usually synthesized by acetylene and isobutanol under certain pressure and temperature. One type of preparation method is that the reaction device adopts an autoclave reactor (see literature: "Zhejiang Chemical Industry", 2006, 12:1-3; Chinese patent 200810062915.X). This method needs to use a large amount of dimethylaniline as a solvent, and the catalyst consumption is very large (8-20% of the weight of isobutanol), resulting in high cost. The autoclave reactor can only be operated intermittently, and for the reaction of acetylene under pressure, it is difficul...

Claims

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Application Information

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IPC IPC(8): C07C43/16C07C41/08
Inventor 黎四芳
Owner XIAMEN UNIV
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