Method for synthesizing trioxymethylene by catalyzing formaldehyde cyclization reaction through bifunctional ionic liquid

A technology of ionic liquid and paraformaldehyde, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low concentration of paraformaldehyde, high equipment requirements, Harsh operating conditions and other issues, to achieve the effect of good repeated use, high product selectivity, and simple operation process

Inactive Publication Date: 2011-04-20
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the sulfuric acid method is generally used in the industry to synthesize paraformaldehyde, which has obvious defects such as strong corrosion of dilute sulfuric acid, high requirements for equipment, large investment, many by-products, and serious environmental pollution.
In recent years, the research on using solid acid instead of protonic acid as catalyst has received great attention. The reported solid acid catalyst system such as ZrO 2 , Zr(OH) 2 、TiO 2 , SnO 2 、Al 2 o 3 (ZSM-20), Y-type zeolite, acidic ion exchange resin, heteropolyacid, etc. 6124480, US 5929257, CN1136812, CN 1162309); Although these catalysts are all effective under certain conditions, one or more defects often exist in the catalytic process, such as harsh operating conditions, longer reaction time and because a large amount of solid supports A large amount of solid waste is generated due to the use of
The above catalyst systems all use more than 60% concentrated formaldehyde as the reaction raw material, which has the disadvantages of low concentration of paraformaldehyde in the synthesis liquid and low product selectivity

Method used

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  • Method for synthesizing trioxymethylene by catalyzing formaldehyde cyclization reaction through bifunctional ionic liquid
  • Method for synthesizing trioxymethylene by catalyzing formaldehyde cyclization reaction through bifunctional ionic liquid
  • Method for synthesizing trioxymethylene by catalyzing formaldehyde cyclization reaction through bifunctional ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A catalytic reaction-rectification device is adopted, wherein the rectification section is a glass packed tower with an inner diameter of 26 mm and a height of 300 mm. The reaction kettle is a 250mL glass three-necked bottle. 200g of 50.0wt.% formaldehyde aqueous solution and 4.0g of ionic liquid 1 were successively added into the reaction kettle. Heating is fully refluxed to be stable, and the reflux ratio R=2 is adjusted, and the azeotrope of formaldehyde, paraformaldehyde and water is steamed from the top of the tower (paraformaldehyde synthesis liquid), and the continuous feed (50.0wt.% Formaldehyde aqueous solution), the feed rate is 20g / h. The temperature of the reaction kettle was controlled at 97-98°C, the temperature at the top of the tower was 92-94°C, and the reaction was carried out for 4 hours to obtain 80g of paraformaldehyde synthesis liquid. The content of each component was analyzed by chromatography and quantified by the internal standard method. The...

Embodiment 2

[0031] Same as Example 1, using ionic liquid 2 as catalyst. The content of paraformaldehyde in the synthesis liquid is 37.0wt.%, the content of formaldehyde is 13.9wt.%, the content of methanol is 0.4wt.%, and the content of formic acid is 182.3ppm. The paraformaldehyde selectivity is 100%.

Embodiment 3

[0033] Same as Example 1, using ionic liquid 3 as catalyst. The content of paraformaldehyde in the synthesis liquid is 18.0wt.%, the content of formaldehyde is 23.8wt.%, the content of methanol is 0.8wt.%, and the content of formic acid is 101.4ppm. The paraformaldehyde selectivity is 100%.

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Abstract

The invention discloses a method for synthesizing trioxymethylene by catalyzing cyclization reaction of aqueous solution of formaldehyde through bifunctional ionic liquid. In the method, the bifunctional ionic liquid is taken as a catalyst, a mode of catalytic rectification reaction is adopted, and the trioxymethylene is prepared through the formaldehyde cyclization reaction. The method has the advantages that: the application range of reaction materials is wide, the catalyst is low in corrosion, high in catalytic activity and recyclable, the product is high in selectivity, and the operating process is simple and high in controllability.

Description

technical field [0001] The invention relates to a method for synthesizing paraformaldehyde by the cyclization reaction of aqueous formaldehyde solution catalyzed by a bifunctional ionic liquid. Background technique [0002] Paraformaldehyde is a white crystal with stable property, low toxicity and easy storage and transportation. It can be used to prepare anhydrous formaldehyde and stabilizer, fumigant, insecticide, molding material, adhesive and disinfectant in color photos. , Antibacterial drugs, etc. At the same time, paraformaldehyde is an important raw material for the synthesis of polyoxymethylene resin. POM has chemical corrosion resistance, high mechanical strength and good plasticity, and is widely used in automobiles, machinery, chemicals, electronics, electrical appliances, instruments and Daily necessities and other fields. With the growth of China's economy, the demand for polyoxymethylene is increasing year by year. The process of synthesizing POM through pa...

Claims

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Application Information

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IPC IPC(8): C07D323/06B01J31/02
CPCY02P20/10Y02P20/584
Inventor 陈静宋河远夏春谷唐中华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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