Preparation method of alkyl glycidyl ether

A technology of glycidyl ether and alkyl, which is applied in the field of preparation of alkyl glycidyl ether, can solve the problems of low yield and low purity, and achieve the effects of high yield, high product purity and simple operation process

Active Publication Date: 2021-01-22
RIANLON ZHONGWEI NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The main purpose of the present invention is to provide a kind of preparation method of alkyl glycidyl ether, to solve the problems of low purity and low yield when preparing alkyl glycidyl ether in the prior art

Method used

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  • Preparation method of alkyl glycidyl ether
  • Preparation method of alkyl glycidyl ether
  • Preparation method of alkyl glycidyl ether

Examples

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preparation example Construction

[0035] In order to make the continuous flow substitution reaction more efficient, in a preferred embodiment, the above-mentioned preparation method comprises the following steps: mixing the alkyl alcohol with the epihalohydrin to form the first raw material liquid; mixing the catalyst with the liquid caustic soda, forming a second raw material liquid; sending the first raw material liquid and the second raw material liquid into a microchannel reactor for continuous flow substitution reaction to obtain alkyl glycidyl ether. In this way, the reaction monomers are mixed in advance, the catalytic gas is mixed, and then passed into the microchannel reactor for reaction, which is conducive to the full contact of each reaction raw material, so as to minimize the reaction time and obtain higher yield.

[0036] In the actual operation process, the first raw material liquid and the second raw material liquid can be placed in two liquid storage units respectively, and then the two raw ma...

Embodiment 1

[0043] Prepared mixed long carbon chain alkyl glycidyl ether in this embodiment, concrete operation is as follows:

[0044] At room temperature (about 25°C), 196g (about 1.0mol) of C 12 -C 14 Add long-chain mixed alkyl alcohol (commercially available), 111g (1.2mol) epichlorohydrin into a single-necked flask, and magnetically stir until the materials are completely mixed to form the first raw material solution; 48g (1.2mol) NaOH, 300ml water and 11g (0.03mol) of ethyltriphenylphosphine bromide were added to a single-necked round-bottomed flask, stirred electromagnetically, until completely mixed to form a second raw material solution;

[0045] Turn on the heat exchange system of the microchannel reactor, set the temperature of the hot oil to 50°C, and start the two feeding pumps A and B after the outlet temperature of the hot oil in the microchannel reactor is 50±0.5°C, and the feeding pump A delivers the first Raw material liquid, feeding pump B transports the second raw ma...

Embodiment 2

[0049] The difference from Example 1 is:

[0050] Turn on the heat exchange system of the microchannel reactor, set the temperature of the hot oil at 60°C to the outlet temperature of the hot oil of the microchannel reactor at 60±0.5°C, and then start two feeding pumps A and B, and the feeding pump A delivers the first raw material Liquid, feeding pump B transports the second raw material liquid. Wherein, the feeding speed of the first raw material liquid and the second raw material liquid is both 20ml / min, the retention time of the material is 1.2min, continuous feeding and continuous discharging.

[0051] Use a 1000ml four-neck round bottom flask to receive the reaction solution, then let the reaction solution stand, separate the lower aqueous phase, add a small amount of water, wash once, carry out vacuum distillation on the organic phase, collect 180-190 ° C fractions (2-3mmHg), The product is a colorless, slightly viscous liquid with a yield of 83% and a gas chromatograp...

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Abstract

The invention provides a preparation method of alkyl glycidyl ether. The preparation method comprises the following steps: carrying out the following continuous flow substitution reaction on alkyl alcohol and epoxy halogenated propane in a micro-channel reactor to obtain alkyl glycidyl ether; wherein the alkyl alcohol comprises one or a mixture of more of compounds CnH<2n+1>OH shown as a formula I, and n in the formula I is 12-14; the epoxy halopropane has a structure shown as a formula II, and X in the formula II is a halogen atom. The invention solves the problems that in the prior art, whenalkyl glycidyl ether is prepared, reaction safety is poor, the number of byproducts is large, and the product yield and purity cannot be considered at the same time; the preparation method is simplein operation process, high in product purity, efficient, safe, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of alkyl glycidyl ether. Background technique [0002] UV-400 is a liquid ultraviolet absorber with excellent performance, mainly used in high-performance coatings and automotive paints, its structure is as follows: [0003] [0004] UV-400 was first successfully developed by Ciba. The two raw materials used in its synthesis are 4,6-bis(2,4-xylyl)-2-(2,4-dihydroxyphenyl)- 1,3,5-triazine, the other is a mixed long carbon chain alkyl glycidyl ether, namely C 12 -C 14 Alkyl glycidyl ether, UV-400 synthetic route is as follows: [0005] [0006] Therefore, want to industrialize the production of ultraviolet absorber UV-400, C 12 -C 14 The production technology of alkyl glycidyl ether must be overcome. [0007] Currently reported C 12 -C 14 The synthetic method of alkyl glycidyl ether is less, as reported a kind of C in the patent CN1014400...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/22B01J19/00
CPCC07D303/22B01J19/0093
Inventor 张会京李宁黄宇范小鹏孙春光李海平
Owner RIANLON ZHONGWEI NEW MATERIAL CO LTD
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