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Application of ionic liquid in synthesis of propylene glycol ether and propylene glycol ether synthesis method

A technology of ionic liquid and propylene glycol ether, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalyst, ether preparation, etc., can solve the problems of difficult recycling and corrosion equipment, and achieve good basic catalysis Effect, low production cost, simple preparation process

Inactive Publication Date: 2016-09-07
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Catalysts commonly used in domestic industry are NaOH, BF 3 , Sodium alkoxide, Potassium alkoxide, but these catalysts all have the disadvantages of corroding equipment and being difficult to recycle.

Method used

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  • Application of ionic liquid in synthesis of propylene glycol ether and propylene glycol ether synthesis method
  • Application of ionic liquid in synthesis of propylene glycol ether and propylene glycol ether synthesis method

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[0016] The present invention also provides a kind of propylene glycol ether synthetic method, described method comprises the steps:

[0017] Feed propylene oxide and alcohol into a reactor to contact with a catalyst, heat to 50°C-200°C in a closed environment to obtain the propylene glycol ether, wherein the catalyst is an imidazole acetate ionic liquid and / or a quaternary ammonium Acetate-like ionic liquids.

[0018] Specifically, the molar ratio of the propylene oxide to alcohol is 1:1-1:10, the molar ratio of the catalyst to propylene oxide is 1:10-1:1000, and the reaction time is 30-300 min. The pressure is usually between 0.1 and 1 MPa. Preferably, the molar ratio of the propylene oxide to alcohol is 1:5-1:4, and the molar ratio of the catalyst to propylene oxide is 1:50-1:200. More preferably, the alcohol is C 1 ~C 8 any of the alcohols.

[0019] The imidazole acetate ionic liquid is at least one of [EMIM][AC], [DMIM][AC] and [BMIM][AC], and the quaternary ammonium ...

Embodiment 1

[0022] Synthesis of Ionic Liquid [N2221][AC]:

[0023] 1.91g of [N2221][MC], 1.2g of acetic acid was reacted in 3mL of water at room temperature for 1 hour and reacted. During the reaction, the methyl carbonate ionic liquid [N2221][MC] reacted with acetic acid to generate water and carbon dioxide, and finally generated [ N2221] [AC], the obtained solvent was washed three times with ether, and then dried in vacuum at 50° C. to obtain yellow crystals.

[0024] Propylene oxide, methanol and [N 2221 ][AC] mixed evenly and sent into the microwave reaction tube, in the microwave reactor, heated to 50 ℃, reacted for 30min. The composition of the obtained liquid phase mixture was measured by gas chromatography, and the conversion rate of propylene oxide was calculated to be 2.5%, and the selectivity of propylene glycol monomethyl ether was 89.6%.

Embodiment 2

[0026] Synthesis of Ionic Liquid [EMIM][AC]:

[0027] Potassium acetate (1.0 mol) was dissolved in 700 mL of anhydrous methanol at 70 °C, and 1-ethyl-3-methylimidazolium bromide [EMIM][Br] (1.0 mol) was dissolved in 100 mL of anhydrous methanol, Subsequently, the potassium acetate solution was added dropwise to the 1-ethyl-3-methylimidazolium bromide acetate solution within 5 minutes. During the dropwise addition process, KBr solids were constantly precipitated. After the dropwise addition was completed, the reaction was carried out for 2 hours. is 70°C. After cooling the complete solution, KBr was removed by filtration, and the filtrate was distilled under reduced pressure to remove anhydrous methanol, and finally obtained light yellow transparent sticky liquid 1-ethyl-3-methylimidazole acetate [EMIM][Ac ].

[0028] Mix propylene oxide, methanol and [EMIM][AC] with a molar ratio of 1:3:0.01 evenly and send them into a microwave reaction tube. In the microwave reactor, heat ...

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Abstract

The invention relates to the technical field of chemical catalysis and provides application of ionic liquid in synthesis of propylene glycol ether and a propylene glycol ether synthesis method. The ionic liquid is imidazole acetate ionic liquid and / or quaternary amine acetate ionic liquid, serves as a catalyst for catalyzing synthesis of the propylene glycol ether. The propylene glycol ether synthesis method includes the following steps that epoxy propane and alcohol are added to a reactor to be in contact with the catalyst, heating is performed in a closed environment to reach 50-200 DEG C, the propylene glycol ether is obtained, wherein the catalyst is the acetate ionic liquid and / or the quaternary amine acetate ionic liquid. The propylene glycol ether synthesis method is a green synthesis process, has not special production equipment requirements and facilitates industrial production and application, and the process is simple and easy to control.

Description

technical field [0001] The invention belongs to the field of chemical catalysis, and in particular relates to the application of ionic liquid in the synthesis of propylene glycol ether and the synthesis method of propylene glycol ether. Background technique [0002] Propylene glycol ether is one of the important industrial derivatives of epoxy compounds, which is mainly produced by the reaction of propylene oxide and alcohols. Since propylene glycol ether has two groups with strong solubility functions-alcohol ether and hydroxyl group, it has a very strong Solubility properties. Known as a universal solvent, it is widely used in coatings, inks, paints, printing, etc. Due to the steric hindrance effect of propylene oxide, the ring-opening position of propylene oxide will be different under the conditions of acid and alkali, and then an addition reaction occurs with alcohols, and the alkali generates 1-methoxy-2-propanol, and The acid produces 2-methoxy-1-propanol. Catalyst...

Claims

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Application Information

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IPC IPC(8): B01J31/04C07C41/03C07C43/10
CPCB01J31/04B01J31/0279B01J31/0284B01J2231/48C07C41/03C07C43/10
Inventor 张锁江刘瑞霞陈圣新张瑞锐赵聪贺滨
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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