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Preparation method of 1,4-dioxane produced by dehydrating ethylene glycol

A technology of dioxane and ethylene glycol, applied in 1 field, can solve the problems of repeated use limitation, poor high temperature resistance, etc., and achieve the effects of easy recycling, mild catalytic performance, and broad industrial application prospects.

Inactive Publication Date: 2018-06-01
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The best experimental conditions are: the volume ratio of ethylene glycol to D72H type dry resin is 10.6:1.0, the reaction temperature is 170°C, the system pressure is 66.7 kPa, and the yield of pure 1,4-dioxane is 95.8%, but the resin is resistant to Poor high temperature performance, limited reuse
[0011] At present, the use of basic catalysts for the dehydration of ethylene glycol to prepare 1,4-dioxane has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Activated carbon was impregnated with KCl, dried at 100 °C for 12 h, and then calcined at 450 °C for 4 h to obtain a catalyst with a loading capacity of 8% KCl / AC.

[0030] The KCl / AC catalyst with a loading of 8% was activated at 300 °C for 2 h.

[0031] In the fixed bed reactor, ethylene glycol is used as the raw material, and the mass space velocity is controlled at 0.3h -1 , the reaction temperature is 200℃, under this condition, ethylene glycol and the activated supported KCl / AC catalyst were reacted for 12 h to obtain 1,4-dioxane.

[0032] Reaction results: The average conversion rate of ethylene glycol was 53%, and the selectivity of 1,4-dioxane was maintained at 60%.

Embodiment 2

[0034] The activated carbon was impregnated with CsCl, dried at 120 °C for 12 h, and then calcined at 450 °C for 4 h to obtain a CsCl / AC catalyst with a loading of 5 wt%.

[0035] The CsCl / AC catalyst with a loading of 5 wt % was activated at 300 °C for 2 h.

[0036] In the fixed bed reactor, ethylene glycol is used as the raw material, and the mass space velocity is controlled at 0.3h -1 , the reaction temperature was 300°C, under this condition, ethylene glycol and the activated CsCl / AC catalyst with a loading of 5% were reacted for 12 h to obtain 1,4-dioxane.

[0037] Reaction results: The average conversion rate of ethylene glycol was 91%, and the selectivity of 1,4-dioxane was maintained at 58%.

Embodiment 3

[0039] Activated carbon was treated with SrCl 2 After impregnation, it was dried at 120 °C for 12 h, and then calcined at 450 °C for 4 h to obtain SrCl with a loading capacity of 15 wt %. 2 / AC Catalyst.

[0040] The catalyst with a loading of 15 wt % was activated at 250 °C for 2 h.

[0041] In the fixed bed reactor, ethylene glycol is used as the raw material, and the mass space velocity is controlled at 0.6h -1 , the reaction temperature is 270 ° C, under this condition, ethylene glycol and activated SrCl with a loading of 15% 2 / AC catalyst for 12 h to obtain 1,4-dioxane.

[0042]Reaction result: The average conversion rate of ethylene glycol is 99%, and the selectivity of 1,4-dioxane is 66%.

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Abstract

The invention relates to a preparation method of 1,4-dioxane produced by dehydrating ethylene glycol. According to the preparation method, activated carbon is used as a carrier, alkali metal salts oralkaline earth metal salts are taken as active components, a catalyst loaded with the active components is prepared after impregnation, and the 1,4-dioxane is prepared by carrying out a dehydration reaction on the ethylene glycol which is used as the raw material. The catalyst used in the method is simple and convenient to prepare, high in activity and good in stability, and still maintains betteractivity after being used for a plurality of times; furthermore, the conversion rate of the ethylene glycol is within a range of 50-99%, and the selectivity of the 1,4-dioxane is within a range of 30-98%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to the preparation technology of 1,4-dioxane catalyst. technical background [0002] 1,4-dioxane (1,4-dioxane), also known as dioxane, is a colorless liquid with a slight fragrance. Density 1.0329, melting point 11°C, boiling point 101.1°C. Miscible with water and many organic solvents. It is often used as a solvent for cellulose acetate, resin, vegetable oil, mineral oil, oil-soluble dyes, etc. It is also used to make spray paint, varnish, plasticizer, wetting agent, nitrocellulose, paint remover, preservative, fragrance, polishing agent , fumigation disinfectants, deodorants and medical supplies. [0003] In industrial production, sulfuric acid or phosphoric acid is mainly used as a catalyst for dehydration reaction to prepare 1,4-dioxane. Although, the catalyzer with sulfuric acid or phosphoric acid as dehydration reaction has advantages such as high cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12B01J27/10B01J27/138
CPCB01J27/10B01J27/138C07D319/12
Inventor 菅盘铭吴发明方思梦张雅云王子豪
Owner YANGZHOU UNIV
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