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Continuous catalytic extraction method for preparing methylal

A technology of methylal and formaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as separation difficulties and achieve the effect of easy separation of products

Active Publication Date: 2019-10-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, formaldehyde cannot react completely, which will still cause great difficulties for subsequent separation, including the separation of water in the reaction mixture and the recovery of formaldehyde.

Method used

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  • Continuous catalytic extraction method for preparing methylal
  • Continuous catalytic extraction method for preparing methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087]The prereactor is a stainless steel fixed bed reactor with an inner diameter of 14mm and a height of 0.3m, filled with 40 ml of strong acidic cation exchange resin catalyst, and the outlet of the prereactor is connected to the heavy phase feed pipe of the catalytic extraction reactor.

[0088] A stainless steel catalytic extraction reactor with an inner diameter of 20mm and a height of 1.3m is filled with 160ml of strongly acidic cation exchange resin catalyst and 200ml of Φ3×3mm stainless steel θ mesh ring, which are evenly mixed. The filling height is 1.2m, and the top 10cm is an empty tube. Set the heavy phase feed pipe at the top of the reactor 1.2m, that is, the top of the catalyst and θ mesh ring bed, set the light phase discharge pipe on the top of the reactor to connect the back pressure valve to control the reaction pressure, and set the light phase feed pipe at the bottom of the reactor , the bottom of the reactor is connected to a temperature-resistant and pres...

Embodiment 2

[0093] Adopt the same prereactor, catalytic extraction reactor, catalyst, catalyst loading method and loading amount as in Example 1.

[0094] 38wt% formaldehyde solution (containing methanol 3wt%), methanol and PODE 2+ (PODE 2 Accounting for 95wt%, PODE 3+ Accounting for 4wt%) enters the prereactor after mixing, and feed rate is respectively 10ml / min, 11ml / min, 0.8ml / min; Alkanes each account for 20wt%) as the extractant, feed from the bottom of the reactor, feed rate 20ml / min; pre-reactor reaction temperature 60 ℃, catalytic extraction reactor reaction temperature 80 ℃, reaction pressure 0.5MPa.

[0095] The output of the light phase at the top of the reactor is 24.7g / min, including 0.13wt% formaldehyde, 0.58wt% methanol, 0.12wt% water, 41.5wt% DMM, PODE 2+ 2.7wt%, and the rest are alkane mixtures and trace by-products.

[0096] The output of the heavy phase at the bottom of the reactor is 9.9g / min, including 0.8wt% methanol, 0.01wt% formaldehyde, 0.06wt% alkane mixture...

Embodiment 3

[0098] Adopt the same prereactor, catalytic extraction reactor, catalyst, catalyst loading method and loading amount as in Example 1.

[0099] 38wt% formaldehyde solution (containing methanol 3wt%), methanol and PODE 2+ (PODE 2 Accounting for 95wt%, PODE 3+ accounted for 4wt%) into the pre-reactor after mixing, the feed rate was 8ml / min, 8.8ml / min, 1ml / min; using toluene and ethylbenzene mixture (weight ratio 1:1) as the extractant, from the bottom of the reactor Feed, the feed rate is 6.3ml / min; the reaction temperature of the pre-reactor is 70°C, the reaction temperature of the catalytic extraction reactor is 60°C, and the reaction pressure is 0.5MPa.

[0100] The output of the light phase at the top of the reactor is 14.8g / min, including 0.18wt% formaldehyde, 0.8wt% methanol, 0.06wt% water, 56.2wt% DMM, PODE 2+ 5.8wt%, and the rest are toluene, ethylbenzene and trace by-products.

[0101] The output of the heavy phase at the bottom of the reactor is 8 g / min, including ...

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Abstract

The invention discloses a method for preparing methylal from a methanol and formaldehyde aqueous solution. The method comprises the following steps that (a) a material A containing formaldehyde and amaterial C containing methanol are introduced into a pre-reactor for pre-reaction, and thus a pre-reaction material I is obtained; and (b) the pre-reaction material I obtained in the step (a) is introduced into a catalytic extraction tower or a multistage catalytic extraction reactor to make countercurrent contact with an extraction agent, and catalytic reaction and extraction are conducted to obtain an extraction phase material II and a raffinate material III. According to the method, the concentration of the methylal in the extraction phase obtained from the catalytic extraction tower can beincreased, and the method has the advantages that the material cost is low, and products are easy to separate.

Description

technical field [0001] The application relates to a continuous catalytic extraction method for preparing methylal from methanol and formaldehyde aqueous solution, which belongs to the field of chemical engineering. Background technique [0002] Methylal, also known as dimethoxymethane, referred to as DMM, the molecular formula is CH 3 OCH 2 OCH 3 , is a colorless, non-toxic and environmentally friendly chemical raw material, usually prepared by aldol condensation reaction of methanol and formaldehyde aqueous solution, the reaction formula is as follows, [0003] [0004] Japanese Asahi Kasei Corporation discloses a catalytic rectification method for producing methylal from formaldehyde aqueous solution and methanol in Chinese patent CN 1020450 C. It adopts the form of a secondary reactor arranged outside the catalytic rectification tower, with macroporous or gel type The cation exchange resin is the catalyst. [0005] Chinese patent CN 102351666 A discloses a catalyti...

Claims

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Application Information

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IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCC07C41/56C07C41/58C07C43/30
Inventor 孙新德刘中民于政锡
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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