Method for preparing aliphatic crown ether from ethylene oxide through oligomerization

A technology of ethylene oxide and aliphatic, which is applied in the field of preparation of aliphatic crown ether by oligomerization of ethylene oxide, which can solve the problems of high market price, need for batch operation, and large equipment occupation, so as to broaden the range of catalysts Types and proportions, reducing equipment material requirements, and avoiding the effect of recycling problems

Pending Publication Date: 2022-07-05
浙江肯特催化材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The Williamson ether synthesis route and its variants have at least the following unfavorable factors, which lead to low selectivity of the cyclization reaction, low yield, many by-products, difficult purification, and batch operation, resulting in high market prices:
[0011] 1. The two ends of dichlorotriethylene glycol or triethylene glycol di-p-toluenesulfonate may condense with different triethylene glycol molecules to form chain polyethers or crown ethers with larger rings, resulting in increased by-products. The property is reduced, and the yield is low;
[0012] 2. Multiple times of complexation and recrystallization are required to obtain 18-crown-6 with sufficient purity, and a large amount of waste with complex components is produced in the process;
[0013] 3. It can only be produced in batches, and the equipment occupies a lot and the production efficiency is low

Method used

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  • Method for preparing aliphatic crown ether from ethylene oxide through oligomerization
  • Method for preparing aliphatic crown ether from ethylene oxide through oligomerization
  • Method for preparing aliphatic crown ether from ethylene oxide through oligomerization

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Embodiment 1: a kind of boron trifluoride catalyzes the method for oligomerization of ethylene oxide into aliphatic crown ether, carries out according to the following steps:

[0056] (1) Preparation of polymerization raw materials:

[0057] Monomer solution: A 500 mL volume steel cylinder was charged with 86.3 g (100 mL) of commercially available ethylene oxide. 258.9g (393mL) of commercially available pressurized liquefied dimethyl ether is stored in a steel cylinder, the outlet of the steel cylinder is connected to a coil, cooled to below -30°C in a -40°C ethanol cooling bath, and then filled with the aforementioned The steel cylinder forms a solution, which is used as a monomer solution after shaking.

[0058] Catalyst solution: 9.0 g (8 mL) of a commercially available boron trifluoride ether solution (weight ratio 1:1.04) was poured into a 100 mL volume cylinder. 81.0g (88mL) of commercially available pressurized liquefied dimethyl ether is stored in a steel cylind...

Embodiment 2

[0065] Embodiment 2: a kind of method that aluminum trichloride catalyzes ethylene oxide oligomerization into aliphatic crown ether, carries out according to the following steps:

[0066] (1) Preparation of polymerization raw materials:

[0067] Monomer solution: A 500 mL volume steel cylinder was charged with 86.3 g (100 mL) of commercially available ethylene oxide. 345.2g (375mL) of commercially available pressurized liquefied methyl chloride is stored in a steel cylinder, the outlet of the cylinder is connected to a coil, cooled to 0°C in a -20°C ethanol cold bath, and then filled into the aforementioned steel cylinder containing ethylene oxide to form a solution , shake well and use it as a monomer solution for later use.

[0068] Catalyst solution: 1.0 g of commercially available anhydrous aluminum trichloride powder and 1.0 g of deionized water were injected into a steel cylinder with a volume of 100 mL. 54.0g (82mL) of commercially available pressurized liquefied meth...

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Abstract

The invention relates to a preparation method, in particular to a preparation method for preparing aliphatic crown ether from ethylene oxide through oligomerization. The method comprises the following steps: monomer solution preparation, catalyst solution preparation, polymerization reaction, reaction termination and product treatment. The synthesis method provided by the invention has the advantages of low raw material cost, continuous synthesis, easy product separation and the like, and is especially suitable for large-scale continuous production.

Description

technical field [0001] The invention relates to a preparation method, in particular to a preparation method for oligomerizing ethylene oxide into aliphatic crown ethers Background technique [0002] Crown ether is a macrocyclic polyether containing multiple epoxy vinyl ether (-CH3-CH3-O-) structural units in the molecule, with surface and interface activity, and can generate stable complexes, thus improving compatibility, It is widely used as phase transfer catalyst, metal ion separation aid, etc. Since Pedersen discovered crown ethers, scholars have changed the structure of crown ethers from various angles and synthesized thousands of new compounds, but almost all of them stayed in the laboratory stage due to low yield and high cost. [0003] Aliphatic crown ethers are crown ethers with only epoxy vinyl ether structural units in the molecule, among which 18-crown ether-6 (1,4,7,10,13,16-hexaoxocyclooctadecane) The structure is relatively simple and is currently the cheape...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D323/00
CPCC07D323/00Y02P20/584
Inventor 方黎锋郑琪王高倪舒乐
Owner 浙江肯特催化材料科技有限公司
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