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Device and method for preparation of high-concentration methylal by partition wall extraction and catalysis

A catalytic preparation, high-concentration technology, applied in chemical instruments and methods, preparation of organic compounds, separation methods, etc., can solve the problems of complex device control, long process flow, low yield per pass, etc., to reduce equipment investment and production Energy consumption, process method is simple, and the effect of avoiding cycle separation

Active Publication Date: 2021-06-15
青岛迈特达新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Methylal-methanol azeotrope pressure swing rectification process is generally used in existing industrial devices to produce high-concentration methylal. Pressure swing rectification does not need to add a third component, and the product will not be polluted, but there is also high energy consumption. 1. The low single-pass yield is due to the high content of methanol in the azeotrope of methanol and methylal, which makes the yield of high-concentration methylal at the bottom of the pressurized rectification tower low, at 0.6-1.5MPaG Under pressure, the mass fraction of methanol in the methylal-methanol azeotrope is about 17-24%. When the methylal containing 8% methanol mass fraction obtained by atmospheric distillation is used as the feed, the pressurized rectification column The maximum single-pass yield of high-concentration methylal is only 53-67%. If the common raw material with a methylal concentration of 86% on the market is used as the feed material, the maximum single-pass yield of high-concentration methylal is only 18-42%. %, a large amount of methylal-methanol azeotrope is circulated, resulting in the disadvantages of high energy consumption for separation and large investment in equipment
[0007] The synthesis reaction of methylal is limited by chemical balance. Generally, the excess of methanol in the feed is controlled to increase the conversion rate of formaldehyde. In traditional high-concentration methylal production equipment, in order to recover excess methanol and ensure the quality of high-concentration methylal products, Generally, 2 to 3 rectification towers are required, the process flow is long, and there are many equipments. In order to reduce the energy consumption of separation, heat exchange equipment is often added for heat integration.

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  • Device and method for preparation of high-concentration methylal by partition wall extraction and catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The formaldehyde aqueous solution containing formaldehyde mass fraction 37% is fed by the formaldehyde aqueous solution feed pipe 1 feed at the rate of 6000kg / h, and the fresh methanol of mass fraction is 99.9% is fed by the methanol feed pipe 2 feed with the speed of 4739.1kg / h, next door The recycled methanol recovered from the top of the sub-column of the extractive catalytic distillation tower T1 is fed by the methanol recovery pipeline 14 at a rate of 470.9kg / h. After mixing, it is firstly preheated to 65°C by the feed preheater E4, and then enters the prereactor R1 through the prereactor feed pipe 4, and the material after the preliminary reaction of the prereactor R1 enters the next door through the reaction mixture conveying pipe 5 At the lower feed port of the main tower of the extractive catalytic distillation tower T1, the circulating process wastewater from the bottom of the next wall extractive catalytic distillation tower T1 is used as the extractant, and e...

Embodiment 2

[0061] The formaldehyde aqueous solution containing formaldehyde mass fraction 44.5% is fed by the formaldehyde aqueous solution feeding pipe 1 at a rate of 3768kg / h, and the fresh methanol with a mass fraction of 99.9% is fed by the methanol feeding pipe 2 at a rate of 3580.5kg / h. The recycled methanol recovered from the top of the sub-column of the extraction catalytic distillation tower T1 is fed by the methanol recovery pipeline 14 at a rate of 1069.5kg / h, and the three streams of formaldehyde solution feed pipe 1, methanol feed pipe 2 and methanol recovery pipeline 14 After mixing, it is firstly preheated to 60°C by the feed preheater E4, and then enters the prereactor R1 through the prereactor feed pipe 4, and the material after the preliminary reaction of the prereactor R1 enters the next door through the reaction mixture conveying pipe 5 At the lower feed port of the main tower T1 of the extractive catalytic distillation tower, the circulating process wastewater from th...

Embodiment 3

[0066] Formaldehyde aqueous solution containing formaldehyde mass fraction 21.7% is fed by formaldehyde aqueous solution feeding pipe 1 at a rate of 7259kg / h, and mass fraction is 99.9% fresh methanol is fed by methanol feeding pipe 2 at a rate of 3362.7kg / h, next door The recycled methanol recovered from the top of the sub-column of the extractive catalytic distillation tower T1 is fed by the methanol recovery pipeline 14 at a rate of 672.3kg / h. After mixing, it is firstly preheated to 70°C by the feed preheater E4, and then enters the prereactor R1 through the prereactor feed pipe 4, and the material after the preliminary reaction of the prereactor R1 enters the next door through the reaction mixture conveying pipe 5 At the lower feed port of the main tower of extractive catalytic distillation tower T1, the circulating process wastewater from the bottom of the T1 tower is used as an extractant, and enters the upper feed port of the T1 main tower from the process waste water c...

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Abstract

The invention discloses a device and method for preparing high-concentration methylal by extraction and catalysis of a partition wall. The method comprises the following steps: a) mixing formaldehyde aqueous solution and excess methanol and preheating them and sending them to a pre-reactor for reaction; extracting agent water and The output of the pre-reactor is not sent to the upper feed port and the lower feed port of the main tower of the next-door extractive catalytic distillation tower; b) formaldehyde and methanol carry out extraction reaction rectification in the main tower of the next-door extractive catalytic rectification tower, High-concentration methylal is obtained at the top of the tower, and residual methanol is obtained at the top of the side tower; c) The water in the raw material and the water generated by the reaction are extracted from the bottom of the next-door extraction catalytic distillation tower, and part of the water is recycled as an extractant The upper feed port of the main tower of the next-door extraction catalytic rectification tower, and the rest of the water is discharged as process wastewater. The invention uses a next-door extraction and catalytic distillation tower to produce high-concentration methylal, uses non-toxic and harmless water as an extraction agent, has a simple process flow, obtains a high-concentration methylal product in one step, and significantly saves separation energy consumption and equipment investment.

Description

technical field [0001] The invention belongs to the technical field of chemical production technology, and in particular relates to a device and method for preparing high-concentration methylal by using a partition extraction catalytic rectification tower. Background technique [0002] Methylal, also known as dimethoxymethane, is a colorless, non-toxic, and environmentally friendly chemical product that can be used as an organic synthesis intermediate, solvent, and diesel additive. It is a chemical that can replace toxic and harmful solvents and reduce air pollution. Environmentally friendly products, as an excellent solvent, it can be widely used in paint coatings, rubber, leather, electronics, industrial cleaning, insecticides, aerosols and other industries. [0003] Industrially, methylal is usually obtained by the reaction of methanol and formaldehyde aqueous solution catalyzed by an acidic catalyst. Since methylal and methanol can form an azeotrope, conventional distill...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/40B01D3/14B01D3/00B01J8/00C07C41/56C07C41/58C07C43/30
CPCB01D3/009B01D3/146B01D3/40B01J8/00C07C41/56C07C41/58C07C43/30Y02P20/10
Inventor 张效龙王志亮
Owner 青岛迈特达新材料有限公司