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New method for preparing 1,3-dioxolane by catalytic condensation

A technology of dioxolane and catalytic condensation, applied in the direction of organic chemistry, can solve the problems of easy pollution of the environment, strong corrosion, and use restrictions, and achieve the effects of high catalytic efficiency, low equipment requirements, and fast reaction rate

Inactive Publication Date: 2011-09-07
TIANJIN JIULIAN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ru 2036919 etc. have reported that ethylene glycol and formaldehyde react in the presence of an acidic catalyst to generate 1,3-dioxolane. The shortcoming of this method is that the commonly used catalyst is an inorganic acid (such as H 2 SO 4 , HCl, p-MeC 6 h 4 SO 3 H, etc.), not only have many side reactions, but also are highly corrosive and easy to pollute the environment, which limits their use.

Method used

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  • New method for preparing 1,3-dioxolane by catalytic condensation

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: the preparation of 1,3-dioxolane

[0021] 4g SiO 2 (100 mesh) and 50 g of 2% phosphotungstic acid aqueous solution were mixed and stirred at room temperature for 10 h, dried at 100 ° C for 12 h after air drying, and then activated in a muffle furnace at 220 ° C for 2 h. That is, a phosphotungstic acid catalyst with a loading capacity of 20% is obtained.

[0022] Mix 62.07g (1.00mol) of ethylene glycol, 108.0g (1.20mol) of paraformaldehyde and 3g of 20% loaded phosphotungstic acid catalyst, heat to 100°C for 3 hours, filter to remove the catalyst and unreacted trimeric Formaldehyde, the resulting liquid is distilled at atmospheric pressure, and the fraction at 71-75°C is collected to obtain the crude product of dioxolane. Distillate, obtained refined dioxolane 63.5g, content 98.5%.

Embodiment 2

[0023] Embodiment 2: the preparation of 1,3-dioxolane

[0024] 7g SiO 2 (100 mesh) and 100 g of 3% phosphotungstic acid aqueous solution were mixed and stirred at room temperature for 12 hours, dried at 120°C for 12 hours after air drying, and then activated in a muffle furnace at 230°C for 3 hours. That is to obtain a phosphotungstic acid catalyst with a loading capacity of 30%,

[0025] Mix 62.07g (1.00mol) of ethylene glycol, 135.0g (1.50mol) of paraformaldehyde and 3g of phosphotungstic acid catalyst with a loading capacity of 30%, heat to 100°C for 3 hours, filter to remove the catalyst and unreacted trimeric Formaldehyde, the resulting liquid is distilled at atmospheric pressure, and the fraction at 71-75°C is collected to obtain the crude product of dioxolane. Distillate, obtained refined dioxolane 65.0g, content 98.5%.

Embodiment 3

[0026] Embodiment 3: the preparation of 1,3-dioxolane

[0027] 6g SiO 2 (100 mesh) and 100 g of 4% phosphotungstic acid aqueous solution were mixed and stirred at room temperature for 13 hours, dried at 130°C for 12 hours after air drying, and then activated in a muffle furnace at 250°C for 3 hours. That is to obtain a phosphotungstic acid catalyst with a loading capacity of 40%,

[0028] Mix 62.07g (1.00mol) of ethylene glycol, 180.0g (2.00mol) of paraformaldehyde with 3.0g of 40% phosphotungstic acid catalyst, heat to 100°C for 3 hours, filter to remove the catalyst and unreacted three Polyoxymethylene, the obtained liquid is distilled under normal pressure, and the fraction at 71-75°C is collected to obtain the crude product of dioxolane. °C fraction, 68.5 g of refined dioxolane was obtained, with a content of 98.5%.

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Abstract

The invention relates to a new method for preparing 1,3-dioxolane by catalytic condensation, which comprises the following step of: enabling glycol and formaldehyde (trioxymethylene, paraformaldehyde or 37% formalin) to be subjected to condensation reaction under the catalysis of silica gel-supported phosphotungstic acid. The 1,3-dioxolane prepared by the method provided by the invention can be used as a solvent of grease, polymers, coatings and bonding agents, an extracting agent of wax and medicaments (vitamins and the like), a solvent for lithium battery electrolytes, a chlorine-based solvent stabilizing agent, a medicament intermediate or the like. The invention has the advantages that the process is simple, the catalytic efficiency is high, the catalyst dose is little, the reaction rate is high, the yield is high, the equipment requirement is low, a catalyst can be easily recovered and can be reused, and large-scale commercialized preparation and production can be realized, thereby meeting the currently increased market demand.

Description

technical field [0001] The invention relates to a novel catalytic condensation preparation method of 1,3-dioxolane. Background technique [0002] 1,3-Dioxolane is used more and more widely because of its strong water solubility and good solvency. Mainly used as solvents, detergents and extractants for oils and polymers, electrolytic solvents for lithium batteries, chlorine-based solvent stabilizers, pharmaceutical intermediates, etc. Ru 2036919 etc. have reported that ethylene glycol and formaldehyde react in the presence of an acidic catalyst to generate 1,3-dioxolane. The shortcoming of this method is that the commonly used catalyst is an inorganic acid (such as H 2 SO 4 , HCl, p-MeC 6 h 4 SO 3 H, etc.), not only have many side reactions, but also are highly corrosive and easy to pollute the environment, so that their use is limited. [0003] Heteropolyacid (HPA) is an oxygen-containing multi-component composed of central atoms (such as P, Si, As, Ge, etc.) and coord...

Claims

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Application Information

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IPC IPC(8): C07D317/12
Inventor 赵国锋陈波卢建华廖文骏梅淑贞
Owner TIANJIN JIULIAN TECH CO LTD
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