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Method for producing 1,3-dioxolane based on reaction-separation coupling

A technology of dioxolane and reaction, which is applied in the direction of organic chemistry, can solve the problems of increasing energy consumption and increasing costs, and achieves the effects of convenient operation, simple equipment, and cost reduction

Active Publication Date: 2011-12-07
Z RIVER GRP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the need to add a large amount of alkyl-substituted benzene for extractive distillation, energy consumption is increased, and the cost of the process is also increased.

Method used

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  • Method for producing 1,3-dioxolane based on reaction-separation coupling
  • Method for producing 1,3-dioxolane based on reaction-separation coupling
  • Method for producing 1,3-dioxolane based on reaction-separation coupling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, figure 1 A circulating pressurized reaction-rectification coupling device is given, including ethylene glycol raw material tank 1, formaldehyde raw material tank 7, feed pump 2, feed pump 37, absorption tower 3, reactive distillation tower 4, condensation Device 6 and reboiler 25 etc.

[0030] A material inlet and a liquid outlet are respectively provided at the bottom of the reactive distillation tower 4 , a side line outlet is arranged at the middle of the reactive distillation tower 4 , and a gas outlet is arranged at the top of the reactive distillation tower 4 .

[0031] The ethylene glycol raw material tank 1 is connected to the inlet of the feed pump 2 through the feed pipe 9, and a shut-off valve 10 is arranged on the feed pipe 9; the outlet of the feed pump 2 is connected to the feed pipe 27. The formaldehyde raw material tank 7 is connected to the inlet of the feed pump 37 through the feed pipe 35, and a stop valve 36 is arranged on the feed pip...

Embodiment 2

[0037] Embodiment 2, a method for producing 1,3-dioxolane based on reaction-separation coupling, using the device described in Embodiment 1, the following steps are carried out in sequence:

[0038] 1), preparatory work:

[0039] There is ethylene glycol in ethylene glycol raw material tank 1; Store 30% (volume concentration) formaldehyde solution in formaldehyde raw material tank 7; Store in advance by 30% (volume concentration) formaldehyde solution and ethyl alcohol at the bottom of reactive distillation column 4 600 mL of raw material composed of diol (the molar ratio of formaldehyde to ethylene glycol is 1:1). Place filler γ-Al at the bottom of reactive distillation column 4 2 o 3 (S BET =275m 2 / g, aperture 4.68nm) 20g, γ-Al is set in the middle part of reactive distillation tower 4 2 o 3 About 300ml.

[0040] γ-Al at the bottom of reactive distillation column 4 2 o 3 It only acts as a reaction catalyst, and the γ-Al located in the middle of the reaction distill...

Embodiment 2～ Embodiment 4

[0060] Change the following reaction conditions among the embodiment 1: the feed rate r of raw material ethylene glycol, the heating power Q of the tower top pressure P of reactive distillation column 4, reboiler 25 and the setting in reactive distillation column 4 Catalyst type, obtain embodiment 2~4, specific data see table 1.

[0061] Table 1, embodiment 2~4 data

[0062]

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Abstract

The invention discloses a method for producing 1,3-dioxolame based on reaction-separation coupling. The method comprises the following steps of: putting solid acid catalysts on the middle part and at the bottom of a reaction rectifying tower (4) serving as a reaction device; making ethylene glycol and a formaldehyde solution with the volume concentration of 30 percent, enter the reaction rectifying tower (4) from a material inlet at the bottom of the reaction rectifying tower (4) and react on the middle part of the reaction rectifying tower (4), wherein the ethylene glycol and the formaldehyde solution serve as raw materials; and making the reaction product, i.e., 1,3-dioxolame flow out of the top of the reaction rectifying tower (4) in a gas form, condensing with a condenser (6) and discharging, wherein the feeding rate of the ethylene glycol serving as a raw material is 40-200 mL / h, the top pressure of the reaction rectifying tower (4) is 0.3-1.0 Mpa, and the heating power of a reboiler (25) is 50-150W. Due to the adoption of the method, reaction and separation of 1,3-dioxolame can be simultaneously realized in a filling tower.

Description

technical field [0001] The invention relates to a preparation method of organic compound 1,3-dioxolane. Background technique [0002] 1,3-dioxolane, its molecular formula: C 3 h 6 o 2 , the pure product is a colorless transparent liquid, widely used in solvents, detergents, and extractants: it can be used as a detergent for metal films; as a solvent for polymers such as PVC and cellulose derivatives; as a solvent for coatings and adhesives Solvent; components of photosensitive liquid and developer; extractant of grease, wax, medicine (vitamins, etc.); solvent for lithium battery electrolyte, etc. [0003] 1,3-dioxolane is mainly prepared by cyclization reaction of ethylene glycol and formaldehyde in the presence of acidic catalysts such as sulfuric acid, trifluoroboric acid, solid acid and heteropoly acid. Pure dioxolane is typically isolated from the reaction mixture by distillation or rectification. [0004] The earliest patent report (West German patent 1914209) obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/12
Inventor 张炜周少东张超陈新志钱超
Owner Z RIVER GRP LTD