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Method for catalytically synthesizing 1,4-dioxane using granular solid super strong acid

A solid super acid, dioxane technology, applied in organic chemistry and other directions, can solve the problems of many by-products, high energy consumption, corrosion equipment and other problems, and achieve the effect of being beneficial to industrial production, reducing energy consumption and saving costs

Inactive Publication Date: 2005-01-26
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of sulfuric acid catalyzed synthesis of 1,4-dioxane are corrosion of equipment, many by-products, troublesome post-processing of products, and easy to cause environmental pollution, etc.
Zeolite molecular sieve fixed bed catalytic synthesis of 1,4-dioxane overcomes the shortcomings of sulfuric acid catalysis, but the catalytic activity of zeolite molecular sieve is relatively low, the catalytic reaction temperature is high, energy consumption is large, and efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add catalyst: In the reactor, add Φ=3~5mm granular SO 4 2- / TiO 2 -SnO 2 -Al 2 o 3 Solid superacid catalyst 120g;

[0025] (2) Heating by resistance wire under the control of temperature controller: heating to raise the temperature to 200°C;

[0026] (3) Introduce nitrogen: take the space velocity as 70cm 3 / min Input nitrogen into the reactor, and keep the catalytic reaction under nitrogen protection all the time;

[0027] (4) Input ethylene glycol: after the air in the reaction system was excluded, input ethylene glycol vapor into the reactor with a weight space velocity of 30g / h;

[0028] (5) Product generation: ethylene glycol is dehydrated under the action of a catalyst to generate a product;

[0029] (6) Product post-treatment: After the above reaction, the product aqueous solution discharged from the outlet of the reactor is condensed through a condensing device, collected in a sub-flask, and then NaCl is added for salting out, and the organic layer a...

Embodiment 2

[0033] (1) Add catalyst: In the reactor, add Φ=3~5mm granular SO 4 2- / ZrO 2 -Al 2 o 3 Solid superacid catalyst 100g;

[0034] (2) Heating by resistance wire under the control of temperature controller: heating to raise the temperature to 240°C;

[0035] (3) Introduce nitrogen: take the space velocity as 80cm 3 / min Input nitrogen into the reactor, and keep the catalytic reaction under nitrogen protection all the time;

[0036] (4) input ethylene glycol: after the air in the reaction system was excluded, input ethylene glycol in the reactor with a weight space velocity of 40g / h;

[0037] (5) Product generation: ethylene glycol is dehydrated under the action of a catalyst to generate a product;

[0038] (6) Product post-treatment: After the above reaction, the product aqueous solution discharged from the outlet of the reactor is condensed by a condensing device, collected in a flask, and then NaCl is added for salting out, and the organic layer and the brine layer are se...

Embodiment 3

[0042] (1) Add catalyst: In the reactor, add Φ=3~5mm granular SO 4 2- / TiO 2 -SnO 2 -Al 2 o 3 Solid superacid catalyst 110g;

[0043] (2) Heating by resistance wire under the control of temperature controller: heating to raise the temperature to 210°C;

[0044] (3) Introduce nitrogen: at a space velocity of 60cm 3 / min Input nitrogen into the reactor, and keep the catalytic reaction under nitrogen protection all the time;

[0045] (4) Input ethylene glycol: after the air in the reaction system was excluded, input ethylene glycol vapor into the reactor with a weight space velocity of 20g / h;

[0046] (5) Product generation: ethylene glycol is dehydrated under the action of a catalyst to generate a product;

[0047] (6) Product post-treatment: After the above reaction, the product aqueous solution discharged from the outlet of the reactor is condensed by a condensing device, collected in a flask, and then NaCl is added for salting out, and the organic layer and the brine l...

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PUM

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Abstract

The synthesis process of 1, 4-dioxane with granular solid superstrong acid as catalyst includes adding catalyst, heating, leading in nitrogen, feeding glycol, producing product, post-treatment of the product, distillation, purification and other steps. The process has the advantages of high catalytic efficiency, low reaction temperature, single material, simple technological process, high yield, high product purity, low cost, etc. and is suitable for industrial production.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing an organic solvent, in particular to a method for catalyzing and synthesizing 1,4-dioxane by using a granular solid superacid. (2) Background technology [0002] 1,4-Dioxane is an organic solvent with a faint ester smell. It is soluble in both water and organic compounds, and is widely used as solvent, medium, extractant, etc. in the manufacture of medicine, cosmetics, spices, special fine chemicals and scientific research. It is worth noting that 1,4-dioxane and SO 3 The formed complex can be used as a sulfating agent in the synthesis of many compounds. [0003] The fine organic chemical raw materials and intermediates handbook (Chemical Industry Press. 1998) edited by Xu Kexun introduced the synthetic method of 1,4-dioxane. Generally, there are three methods for synthesizing 1,4-dioxane: taking ethylene glycol as raw material and dehydrating under sulfuric acid catalysis; using ethylene oxide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12
Inventor 高根之赵斌
Owner QUFU NORMAL UNIV