Catalysis system for synthesizing methyl propionate and application method thereof

A catalytic system, a technology of methyl propionate, applied in catalytic reactions, chemical instruments and methods, carbon monoxide or formate reaction preparation, etc., can solve the problems of high production cost, harsh reaction conditions, easy decomposition, etc., and achieve recycling good performance, improve catalytic activity and shorten the reaction time

Active Publication Date: 2018-12-14
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Germany's Reppe has proposed ethylene hydroesterification method to directly synthesize methyl propionate or ethyl propionate technology, and it uses Ni series catalyst, and reaction condition is harsh, and equipment requirement is higher; Patent (CN87110635) relates to palladium (II)/ The aryl-substituted phosphine/acid catalyst system has higher activity in catalyzing ethylene/methanol carbonylation, but the phosphine ligand in this kind of ligand system is easy to decompose and cause catalyst deactivation; literature (R.F.Heck, J.A.m.Chem.Soc., 1963,85; W.Keim.J.Mol.Catal.,1989,54(1)) showed that complex catalysts such as ruthenium, nickel, cobalt, etc. were active in oxo-synthesizing met

Method used

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  • Catalysis system for synthesizing methyl propionate and application method thereof
  • Catalysis system for synthesizing methyl propionate and application method thereof
  • Catalysis system for synthesizing methyl propionate and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh Ionic liquid (1) 5.6mmol, Ru 3 (CO) 12 Add 0.042 mmol into the reaction kettle, seal the reaction kettle, put the reaction kettle into an oil bath at a temperature of 70°C, and vacuumize for 0.5h. Add 5.6ml (150mmol) of methanol and 2mmol of ethylene into the reaction kettle under the protection of argon, and fill with CO 2 4MPa and equilibrate the pressure for 3min, the temperature of the reactor was raised to 200°C, the stirring speed was 500r / min, and the reaction lasted for 6h. After the reaction, the liquid in the kettle was orange-red transparent liquid, and the yield of methyl propionate was 98.9%. The test method of the yield: remove the transparent liquid in the reaction kettle into a 10ml vial, add a certain mass of n-heptane into the vial as an internal standard, record the mass of n-heptane added, and calculate the amount of n-heptane by the internal standard method of gas chromatography. The yield of methyl esters.

Embodiment 2

[0044] Others are the same as in Example 1, except that the reaction temperature is 160° C., the reaction time is 20 h, and the yield of methyl propionate is 99.7%. Under the same conditions in the literature, the synthetic yield of methyl propionate is 76.0%.

Embodiment 3

[0046] Others are the same as in Example 1, except that the Ionic liquid (1) is replaced by the ionic liquid [Bmim]Cl in the literature, and the yield of methyl propionate is 37.2%.

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Abstract

The invention discloses a catalysis system for synthesizing methyl propionate and an application method thereof. The catalysis system is prepared from a ruthenium-cluster carbonyl complex, imidazoliumionic liquid and an inorganic salt accelerator, or the ruthenium-cluster carbonyl complex and the imidazolium ionic liquid, wherein the mole ratio of the imidazolium ionic liquid to the ruthenium-cluster carbonyl complex is (100-250):1; when the catalysis system comprises the accelerator, the mole ratio of the accelerator to the ruthenium-cluster carbonyl complex is (1-75):1; the accelerator is carbonate, halogenated lithium or transitional metallic chloride. The system uses the imidazolium ionic liquid to consume water produced in the reaction to accelerate the reaction to be performed towards the forward direction; by the adding of the inorganic salt accelerator, the catalytic activity is further improved, so as to catalyze ethylene, CO2 and methanol to prepare the methyl propionate. The catalysis system obviously shortens the reaction time, so that the yield of the methyl propionate is increased.

Description

Technical field: [0001] The invention belongs to the field of organic chemical products synthesized by hydroesterification reaction, and in particular relates to a method for synthesizing methyl propionate through ethylene carbonylation. Background technique: [0002] Methyl propionate is a colorless and transparent organic liquid, which can be used as spices, solvents, extractants, organic intermediates and plasticizers, and is widely used in adhesives, coatings, textiles, rubber, plastics and other industries . Methyl propionate can produce propionate, propionic acid, propionate (benzyl propionate, isoamyl propionate, etc.) and other products through esterification reaction, hydrolysis reaction and transesterification reaction, so methyl propionate The development of ester synthesis process is beneficial to the progress and development of propionic acid, propionate, propionate and other process technologies. [0003] Germany's Reppe has proposed ethylene hydroesterificat...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C67/38C07F7/18C07C69/24
CPCB01J31/26B01J2231/321C07C67/38C07C69/24
Inventor 刘宾元董甜丽段中余康裕杨立平
Owner HEBEI UNIV OF TECH
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