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A kind of method of synthesizing trioxane

A technology of paraformaldehyde and paraformaldehyde, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve low TOX yield, high production energy consumption, latent heat of vaporization advanced questions

Inactive Publication Date: 2017-12-12
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But no matter what type of catalyst is used, the biggest problem of these methods for synthesizing TOX based on formaldehyde aqueous solution is that the formaldehyde solution needs to be concentrated to more than 50% (the concentration of the formaldehyde solution used in the examples of the above-mentioned patent documents is all greater than 50%) , and the TOX productive rate in the reaction phase is very low (the equilibrium productive rate of TOX in the reactor liquid is only about 2.5% and 1.8% respectively when the above-mentioned conditions are catalyzed with sulfuric acid and ionic liquid, mass percentage), simultaneously formic acid, formic acid Formation of methyl esters, etc., so reactive distillation process must be used to produce TOX
As we all know, the latent heat of vaporization of water is very high, therefore, the separation energy consumption of the above-mentioned process is very high, and most of the energy consumption required for preparing TOX is used for evaporating water (see Mosamoto, J., etal.Synthesis of trioxane using heteropolyacids ascatalyst. Angew.Chem.Int.Ed.2000,39,2102)
On the other hand, the biggest problem of POM engineering plastics is the high energy consumption of production (see Zhang Xinggang for details, and then look at the "Great Leap Forward" of the POM industry. Chemical Management 2011, December, 43), and 75% of the energy consumption comes from monomers Production of TOX (see Grützner, T., et al. Chem. Eng. Sci. 2007, 62, 5613 for details)
At the same time, this type of process also generally has the problem of recovery and treatment of dilute formaldehyde. The recovery of dilute formaldehyde basically adopts a distillation scheme, which has a large recovery volume, high energy consumption, high requirements on equipment materials, and large investment (see Zhang Xinggang for details; see polyoxymethylene again. Industry "Great Leap Forward"; Chemical Management 2011,12,43)

Method used

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  • A kind of method of synthesizing trioxane
  • A kind of method of synthesizing trioxane
  • A kind of method of synthesizing trioxane

Examples

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Embodiment 1

[0072] This embodiment provides a method for synthesizing paraformaldehyde, using ionic liquid as a solvent and catalyst to synthesize paraformaldehyde from solid paraformaldehyde, the specific steps are as follows:

[0073] Preparation of ionic liquid a: Add an appropriate amount of N-methylimidazole to a three-necked flask, slowly add equimolar 1,3-propane sultone dropwise, stir and react for 24 hours, filter with suction to obtain a white precipitate, wash with acetone, vacuum Dry to obtain the intermediate; then add the intermediate to a three-necked flask, dropwise add equimolar concentrated sulfuric acid, use ethyl acetate as a solvent, heat up to 70°C, stir and reflux for 48 hours, then wash with ethyl acetate, and dry in vacuo to obtain ions liquid a.

[0074] Preparation of paraformaldehyde: Add 6.0 g of paraformaldehyde and 30.2 g of ionic liquid a into a 50 mL reactor in sequence, control the reaction temperature at 90° C., and react for 25 minutes to obtain parafor...

Embodiment 2

[0082] This embodiment provides a method for synthesizing paraformaldehyde, using ionic liquid as a solvent and catalyst to synthesize paraformaldehyde from solid paraformaldehyde, the specific steps are as follows:

[0083]Preparation of ionic liquid b: Weigh an appropriate amount of N-methylimidazole and add it to a three-necked flask, slowly add equimolar n-bromobutane dropwise, stir and react for 48 hours, then filter with suction to obtain a white precipitate (intermediate) and wash it with acetone and vacuum dried. Then add the intermediate to the three-necked flask, dropwise add equimolar concentrated sulfuric acid, use ethyl acetate as solvent, heat up to 70°C, stir and reflux for 48 hours, then wash with ethyl acetate, and vacuum dry to obtain ionic liquid b.

[0084] Preparation of paraformaldehyde: add 4.0 g of paraformaldehyde and 30.1 g of ionic liquid b into a 50 mL reaction kettle in sequence, control the reaction temperature at 90° C., and react for 25 minutes ...

Embodiment 3

[0086] This embodiment provides a method for synthesizing paraformaldehyde, using ionic liquid as a solvent and catalyst to synthesize paraformaldehyde from solid paraformaldehyde, the specific steps are as follows:

[0087] Preparation of ionic liquid c: Add an appropriate amount of N-methylimidazole to a three-necked flask, slowly add concentrated sulfuric acid dropwise at a molar ratio of 1:1 under stirring conditions, then gradually raise the temperature to 80°C, react for 3 hours, and reduce the temperature at 0.1MPa at 70°C Distilled under pressure for 0.5h, washed with ethyl acetate, and dried in vacuo to obtain ionic liquid c.

[0088] Preparation of paraformaldehyde: sequentially add 6.1g of solid paraformaldehyde and 31.6g of ionic liquid c into a 50mL reactor, control the reaction temperature at 90°C, and react for 45min to obtain paraformaldehyde; use chromatography to analyze the product in the reactor The concentration of paraformaldehyde was found to be 6.9%, an...

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Abstract

The invention provides a method for synthesizing trioxane. The method comprises the steps of using ionic liquid as solvent and catalyst, using solid paraformaldehyde as raw material, and reacting at 30°C-150°C for 0.1h-5h to synthesize paraformaldehyde, wherein the amount of solid paraformaldehyde is ionic liquid and solid Less than 80% of the total mass of paraformaldehyde. The method provided by the present invention uses solid paraformaldehyde as raw material, and ionic liquid is as solvent and catalyst, can not generate by-product methyl formate, methanol and methylal etc., can significantly improve the equilibrium productive rate of paraformaldehyde, can reduce Energy consumption is low, and the ionic liquid can be reused, thereby reducing production costs.

Description

technical field [0001] The invention relates to a method for synthesizing paraformaldehyde, in particular to a method for synthesizing paraformaldehyde from solid paraformaldehyde by using an ionic liquid as a solvent and a catalyst, and belongs to the technical field of chemical synthesis. Background technique [0002] Paraformaldehyde (TOX) and many related industries are extremely important links in the carbon-one chemical industry chain. First of all, TOX is the raw material for the preparation of polymethoxy dimethyl ether (DMM3-8), and DMM3-8 is an internationally recognized new type of environmentally friendly fuel oxygen-containing component that reduces fuel consumption and smoke emissions, and is internationally recognized The new environment-friendly diesel blending component has a cetane number as high as 76, an oxygen content of 47%-50%, no sulfur and no aroma, and the blending amount can account for 10%-20% of the diesel amount, which can significantly reduce t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D323/06B01J31/02
Inventor 胡玉峰陈禹霏孙宇张海荣黄和志齐建光于永
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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