Method for preparing 1, 4-dioxane

A technology of dioxane and dimethyl ether, applied in the field of solid acid catalysis, to achieve the effects of highlighting environmental friendliness, avoiding environmental pollution, and eliminating industrial wastewater

Inactive Publication Date: 2016-10-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, there are many shortcomings in the traditional 1,4-dioxane preparation process
In particular, it is still impossible to essentially avoid the production of industrial waste water containing trace amounts of dioxane

Method used

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  • Method for preparing 1, 4-dioxane
  • Method for preparing 1, 4-dioxane
  • Method for preparing 1, 4-dioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The H-ZSM-5 molecular sieve with a silicon-aluminum ratio of Si / Al=50 is pressed into tablets under a pressure of 40 MPa and crushed to 20-40 mesh to obtain a catalyst.

[0057] 1 g of catalyst was filled into a fixed bed reactor for pretreatment. Catalyst pretreatment conditions are: N 2 The flow rate is 30ml / min, rising from 25°C to 500°C over 150min, and maintaining at 500°C for 180min.

[0058] The reaction raw material ethylene glycol dimethyl ether is under the condition of water bath temperature 40 ℃, by N 2 Bring it into the reactor at a flow rate of 30ml / min, and the space velocity is 0.08h -1 , The reaction pressure is 3.0Mpa.

[0059] Raw material conversion rate and product selectivity change with temperature as shown in figure 1 shown. From figure 1 It can be seen in the figure that on the H-ZSM-5 (Si / Al=50) catalyst, when the reaction temperature is lower than 80°C, the conversion of raw materials is lower than 40%. However, as the reaction temperat...

Embodiment 2

[0061] The hydrogen-type mordenite with a silicon-aluminum ratio of Si / Al=14.5 was pressed into tablets under a pressure of 40 MPa and crushed to 20-40 mesh to obtain a catalyst.

[0062] 1 g of catalyst was filled into a fixed bed reactor for pretreatment. The pretreatment condition is: N 2 The flow rate is 30ml / min, rising from 25°C to 500°C over 150min, and maintaining at 500°C for 180min.

[0063] The reaction raw material ethylene glycol dimethyl ether is under the condition of water bath temperature 40 ℃, by N 2 Bring it into the reactor at a flow rate of 30ml / min, and the space velocity is 0.4h -1 , The reaction pressure is 0.5Mpa.

[0064] Raw material conversion rate and product selectivity change with temperature as shown in figure 2 shown. From figure 2 It can be seen that when hydrogen-type mordenite (Si / Al=14.5) is used as the catalyst, the conversion rate of raw materials gradually increases with the increase of reaction temperature. At 200°C, the convers...

Embodiment 3

[0066] The H-Beta molecular sieve with a silicon-aluminum ratio of Si / Al=16 was pressed into tablets under a pressure of 40 MPa and crushed to 20-40 mesh to obtain a catalyst.

[0067] 1 g of catalyst was filled into a fixed bed reactor for pretreatment. The pretreatment conditions are: N2 flow rate 30ml / min, starting from 25°C over 150min to 500°C, and maintaining at 500°C for 180min. The reaction raw material ethylene glycol dimethyl ether was prepared by N 2 Bring it into the reactor at a flow rate of 30ml / min, and the space velocity is 0.05h -1 , The reaction pressure is 5.0Mpa.

[0068] Raw material conversion rate and product selectivity change with temperature as shown in image 3 shown. From image 3 It can be seen that when using H-Beta (Si / Al=16) as a catalyst, the conversion rate of the raw material can reach 60% at a lower room temperature (25°C); when the reaction temperature is higher than 50°C, the raw material The conversion rate of ethylene glycol dimeth...

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Abstract

The invention provides a method for preparing anhydrous high-purity 1, 4-dioxane from glycol dimethyl ether through one step. Through the method, high-purity 1, 4-dioxane is prepared from the glycol dimethyl ether raw material at a low temperature at a high conversion rate. In the whole reaction process, water does not react and product water is not produced so that 1, 4-dioxane-containing industrial wastewater is prevented thoroughly. The glycol dimethyl ether raw material has a high conversion ratio at a low temperature, catalyst stability is good, product 1, 4-dioxane selectivity is high and the whole process is simple and environmentally friendly.

Description

technical field [0001] The application belongs to the field of solid acid catalysis, in particular, it relates to a method for preparing 1,4-dioxane. Background technique [0002] 1,4-Dioxane (1,4-Dioxane), also known as dioxane in Chinese, is a colorless and transparent flammable liquid with a faint ester smell, which can form an azeotropic mixture with water. 1,4-Dioxane is widely used in industry. As a solvent, it has excellent solubility properties. Its solubility is similar to that of dimethylformamide and stronger than that of tetrahydrofuran. It can be used as a solvent for cellulose acetate, various resins, vegetable oils, mineral oils, soluble dyes, etc. It is widely used as a reaction medium and volatile solvent in the reactions of polyurethane synthetic leather and amino acid synthetic leather. 1,4-Dioxane is also used as an extractant and reaction medium in the pharmaceutical and fine chemical industries; as a solvent and dispersant in coatings and dyes; in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
Inventor 石磊朱文良倪友明刘红超刘勇刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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