Preparation method of electronic grade propylene glycol monomethyl ether and product thereof

A propylene glycol monomethyl ether, electronic grade technology is applied in the preparation field of electronic grade propylene glycol monomethyl ether, can solve the problems of high catalyst activity and selectivity, low catalyst activity and selectivity, harsh reaction conditions, etc. By-products, beneficial to activation and ring opening, and the effect of stable reactivity

Active Publication Date: 2021-02-26
HAIKE GRP RES INST OF INNOVATION & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the technical problems of harsh reaction conditions for preparing propylene glycol monomethyl ether in the above-mentioned background technology, low catalyst activity and selectivity, and low product purity, and provides a method for preparing electronic grade propylene glycol monomethyl ether and the product obtained therefrom. The reaction conditions are mild, the prepared product has high purity, high yield, and high catalyst activity and selectivity

Method used

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  • Preparation method of electronic grade propylene glycol monomethyl ether and product thereof

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preparation example Construction

[0024] The invention provides a kind of preparation method of electronic grade propylene glycol monomethyl ether, comprises the steps:

[0025] 1) Mix methanol, propylene oxide and alkaline ionic liquid catalyst, and react in a microchannel reactor to obtain a reaction liquid;

[0026] 2) Delighting the reaction solution in step 1) to obtain a delightening reaction solution;

[0027] 3) Evaporate the light-removing reaction solution in step 2), and perform negative pressure distillation on the obtained steam to obtain electronic grade propylene glycol monomethyl ether.

[0028] The invention mixes methanol, propylene oxide and alkaline ionic liquid catalyst, and reacts in a microchannel reactor to obtain a reaction liquid. In the present invention, the molar ratio of methanol to propylene oxide is preferably (2-11):1, more preferably 5:1. In the present invention, the cation of the basic ionic liquid catalyst is preferably 1,3-dialkylimidazolium cation, alkylimidazolium cati...

Embodiment 1

[0050] Inject propylene oxide, methanol and alkaline ionic liquid catalyst (1-butyl-3 methylimidazolium bicarbonate) into the raw material mixer through a metering pump (the feed rate of propylene oxide is 14Kg / h, the feed rate of methanol 23Kg / h, the amount of alkaline ionic liquid catalyst added is 0.5% of the mass of the raw material), multiple raw materials are mixed by the raw material mixer and then enter the raw material preheater, and the raw material preheater preheats the material to 50°C before entering the microchannel reaction The reaction is carried out in the reactor (control the temperature in the microchannel reactor at 100°C, the pressure is 0.3MPa, and the material residence time is 6min), and the gas chromatograph is used to detect and analyze the reaction solution (under the selected chromatographic conditions, the sample gasifies and passes through the chromatographic column , to separate the components therein. Detect with a hydrogen flame detector, calcu...

Embodiment 2

[0059] Propylene oxide, methanol and alkaline ionic liquid catalyst (1-butyl-3 methylimidazole hydroxide) are respectively injected into the raw material mixer through a metering pump (the feed rate of propylene oxide is 14Kg / h, and the feed rate of methanol is 30Kg / h, the amount of alkaline ionic liquid catalyst added is 1.5% of the mass of the raw material), multiple raw materials are mixed by the raw material mixer and then enter the raw material preheater, and the raw material preheater preheats the material to 50 °C before entering the microchannel reactor Fully react within the microchannel reactor (control the temperature in the microchannel reactor at 120°C, the pressure at 0.2MPa, and the material residence time for 3 minutes), and use a gas chromatograph to detect and analyze the reaction solution. The PO conversion rate is greater than 99%, and the isomer selectivity is greater than 98%. .

[0060] Transfer the obtained reaction liquid to the dealcoholization tower...

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Abstract

The invention discloses a preparation method of electronic grade propylene glycol monomethyl ether and a product obtained by the preparation method, and belongs to the technical field of preparation of fine chemicals. The method comprises the following steps of: 1) mixing methanol, propylene oxide and a basic ionic liquid catalyst, and carrying out reaction in a micro-channel reactor to obtain a reaction solution; 2) removing light components from the reaction solution to obtain a light component removed reaction solution; and 3) evaporating the light component removed reaction solution obtained in step 2), and performing negative pressure rectification on the obtained steam to obtain the electronic grade propylene glycol monomethyl ether. The preparation method of the electronic grade propylene glycol monomethyl ether provided by the invention are mild in reaction conditions, the purity of the prepared product is high, the yield is high, and the activity and selectivity of the catalyst are high.

Description

technical field [0001] The invention relates to the technical field of preparation of fine chemicals, in particular to a method for preparing electronic-grade propylene glycol monomethyl ether and a product obtained therefrom. Background technique [0002] Propylene glycol monomethyl ether (PM) is a solvent with excellent performance and low toxicity. It has the characteristics of strong solvency, low volatility and high flash point. Electronic grade propylene glycol monomethyl ether is mainly used in TFT-LCD photoresist diluent, photoresist remover, stripper, IC cleaning agent, photoresist removal buffer, etching process, etc. in the production process of liquid crystal display and photoresist And other chemical products that require special specifications. At the same time, it is widely used as a solvent for the production of electronic materials. The molecular structure and physicochemical properties of PM are similar to glycol ethers, and it is considered to be an idea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/03C07C41/40C07C41/42C07C43/13B01J31/02B01J19/00
CPCB01J19/0093B01J31/0284B01J2219/00889B01J2231/44C07C41/03C07C41/40C07C41/42C07C43/13
Inventor 张在忠魏娟马俊青张勇李荣
Owner HAIKE GRP RES INST OF INNOVATION & TECH
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