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A kind of extractive catalytic rectification method for preparing methylal

A technology of catalytic rectification and catalytic rectification tower, which is applied in the field of extractive catalytic rectification, can solve the problems of high energy consumption and large reflux ratio, and achieve the effects of low energy consumption, reduced reflux ratio and improved product purity

Active Publication Date: 2020-08-07
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

At present, catalytic distillation technology is generally used to break the limitation of chemical balance, but it requires a large reflux ratio and high energy consumption

Method used

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  • A kind of extractive catalytic rectification method for preparing methylal
  • A kind of extractive catalytic rectification method for preparing methylal
  • A kind of extractive catalytic rectification method for preparing methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Such as figure 2 As shown, the catalytic rectification column includes an overhead condensing reflux device, a rectification section, a reaction section, a stripping section and a tower still. The inner diameter of the tower body is 50 mm, the effective height of the rectification section and stripping section is 0.57 meters, and it is filled with Φ3×3 mm stainless steel θ mesh rings. The effective height of the reaction section is 0.97 meters, filled with 15 stainless steel wire mesh bags and 1300 ml Φ5×5 mm stainless steel θ mesh rings that are evenly mixed, and 500 ml of Nafion-H resin is installed in the stainless steel wire mesh bags as a catalyst.

[0062] The feed rate of formaldehyde solution is 14ml / min, the feed temperature is 40°C, and the feed is 40 cm from the upper end of the rectification section; the feed amount of methanol is 15.2ml / min, the feed temperature is 60°C, and the feed is fed from the lower end of the reaction section; The extractant adopts...

Embodiment 2

[0064] Such as figure 2 As shown, the catalytic rectification column includes an overhead condensing reflux device, a rectification section, a reaction section, a stripping section and a tower still. The inner diameter of the tower body is 50 mm, the effective height of the rectification section and stripping section is 0.57 meters, and it is filled with Φ3×3 mm stainless steel θ mesh rings. The effective height of the reaction section is 0.97 meters, filled with 15 stainless steel wire mesh bags and 1300 ml of Φ5×5 mm stainless steel θ mesh rings mixed uniformly, and 500 ml of D005 strong acid cation exchange resin is installed in the stainless steel wire mesh bags as a catalyst.

[0065] The feed rate of formaldehyde solution is 14ml / min, the feed temperature is 40°C, and the feed is fed from the upper end of the rectification section 40 cm down; the feed amount of methanol is 15.4ml / min, the feed temperature is 60°C, and the feed is fed from the lower end of the reaction s...

Embodiment 3

[0067] Such as figure 2 As shown, the catalytic rectification column includes an overhead condensing reflux device, a rectification section, a reaction section, a stripping section and a tower still. The inner diameter of the tower body is 50 mm, the effective height of the rectification section and stripping section is 0.57 meters, and it is filled with Φ3×3 mm stainless steel θ mesh rings. The effective height of the reaction section is 0.97 meters, filled with 15 stainless steel wire mesh bags and 1300 ml of Φ5×5 mm stainless steel θ mesh rings mixed uniformly, and 500 ml of D005 strong acid cation exchange resin is installed in the stainless steel wire mesh bags as a catalyst.

[0068] Dilute the analytically pure formaldehyde aqueous solution reagent with water until the formaldehyde content is 10wt% as the reaction raw material, wherein the methanol content is diluted to 0.78wt%. The feed rate of 10wt% formaldehyde aqueous solution is 46.5ml / min, the feed temperature i...

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Abstract

An extractive catalytic rectification method for preparing methylal from methanol and formaldehyde aqueous solution, comprising: preparing methylal from methanol and formaldehyde aqueous solution in a catalyst rectification tower, said catalytic rectification tower comprising a reaction section and a rectification section, The solid catalyst A is filled in the reaction section; methanol and formaldehyde aqueous solution are introduced into the catalytic rectification tower, and contact with the solid catalyst A in the reaction section to obtain methylal; the solid catalyst A is a solid acid catalyst; The above reaction section contains an extractant. Compared with the traditional catalytic distillation process, it has the advantages of low content of methanol and formaldehyde in the methylal product, high purity of the methylal product, and low energy consumption.

Description

technical field [0001] The invention relates to an extraction catalytic rectification method for preparing methylal from methanol and formaldehyde aqueous solution. Background technique [0002] Methylal, also known as dimethoxymethane, has the molecular formula CH 3 OCH 2 OCH 3 , is a colorless, non-toxic and environmentally friendly chemical raw material. It is 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 catalytic rectification method for the continuous production of high-c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCY02P20/10
Inventor 孙新德刘中民于政锡
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI