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C-4 based method for preparing mma with recovery and recycling of methacrolein

A technique for fractionation of methacrolein and methacrolein, applied in the field of preparation of methacrylate, can solve problems such as safety problems, insufficient compensation, pressure and temperature rise, etc., achieve low cost and increase catalyst utilization Effect

Pending Publication Date: 2022-02-18
ROHM G M B H
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These in turn can lead to spontaneous pressure and / or temperature increases which are problematic in terms of safety
[0024] 4) Last but not least, methacrolein cannot be fully converted in the second reaction zone
However, all these solutions have a common feature that they can only be implemented through complex and expensive measures
Also, many problems cannot be adequately compensated, especially in continuous operation

Method used

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  • C-4 based method for preparing mma with recovery and recycling of methacrolein
  • C-4 based method for preparing mma with recovery and recycling of methacrolein
  • C-4 based method for preparing mma with recovery and recycling of methacrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0144] corresponding to figure 1 In the setup of , a process gas feed (PG1) containing isobutene (F3) as starting material, air (F1), a cycle gas stream containing oxygen and inert gases ( F2) and Steam (F4). The stream has an overall molar ratio of isobutene to oxygen to water of 1:2:1.5. The temperature in the reactor was maintained at 350°C and the pressure at the reactor inlet was maintained at a positive pressure of 1.2 bar. This results in 1.000h -1gas hourly space velocity (GHSV). The reaction was carried out in a tube bundle reactor using a molybdenum oxide based catalyst prepared according to US2007 / 0010394. The resulting process gas (PG2) having a temperature of 343°C is obtained. This process gas has the following composition: 4.8 vol % methacrolein, 0.74 mol % CO, 0.21 mol % methacrylic acid, 0.21 mol % acetic acid, 0.12 mol % acetone, 0.21 mol % acetaldehyde, 0.04 mol % acrolein, 0.03 mol % formaldehyde, 0.03 mol % acrylic acid, 250 ppm isobutylene and 3.5 ...

Embodiment 2

[0154] The isobutene oxidation was carried out in a similar manner to Example 1, but with a modified composition of the recycled methacrolein-containing gas mixture (PG6). Streams F1, F2, F4 and PS4 were adjusted such that the process gas (PG6) had the following composition: 1.40 mol % methacrolein, 0.03 mol % methacrylic acid, 0.09 mol % acetone, 0.05 mol % acetone Aldehyde, 0.04 mol% acrolein, 17.1 mol% oxygen and 13.5 mol% water. As in Example 1, process gas PG6 at a temperature of 80°C is passed into distributor (G1) and mixed with process gas (PG2) to form process gas (PG3) at a temperature of 240°C, however, the process gas (PG3) has a ratio of methacrolein, oxygen and water in a ratio of 1 / 2.8 / 4.1, and contains a total of 4.44 mol% of organic components. The organic components are as follows: 3.31mol% methacrolein, 0.30mol% CO, 0.12mol% methacrylic acid, 0.12mol% acetic acid, 0.15mol% acetone, 0.15mol% acetaldehyde, 0.06 mol % acrolein, 0.02 mol % formaldehyde and 0.0...

Embodiment 3

[0157]The isobutene oxidation was carried out in a similar manner to Example 1, but with a modified composition of the recycled methacrolein-containing gas mixture (PG6). Streams F1, F2, F4 and PS4 were adjusted such that the process gas (PG6) had the following composition: 1.40 mol % methacrolein, 0.03 mol % methacrylic acid, 0.09 mol % acetone, 0.05 mol % acetonitrile Aldehyde, 0.04 mol% acrolein, 10 mol% oxygen and 13.5 mol% water. As in Example 1, process gas PG6 at a temperature of 80°C is passed into distributor (G1) and mixed with process gas (PG2) to form process gas (PG3) at a temperature of 240°C, however, the process gas (PG3) has a ratio of methacrolein, oxygen and water in a ratio of 1 / 2 / 4.1, and contains a total of 4.44 mol % of organic components. The organic component is composed of 3.31 mol% methacrolein and 0.30 mol% CO, 0.12 mol% methacrylic acid, 0.12 mol% acetic acid, 0.15 mol% acetone, 0.15 mol% acetaldehyde, 0.06 mol % acrolein, 0.02 mol % formaldehyde...

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Abstract

The present invention describes an improved process for the preparation of methacrylic acid esters, in particular methacrylic acid and methyl methacrylate (MMA), based on C-4 raw materials. In this case, the C4 feedstock is in particular isobutene or tert-butyl alcohol. In addition, a wide range of embodiments for efficiently preparing these products are also provided. The invention relates in particular to a method for producing methacrylic acid and methyl methacrylate by gas-phase oxidation of isobutene. In a second gas phase oxidation step, methylacrolein is converted into methacrylic acid and unconverted methylacrolein is removed from methacrylic acid. This methacrolein is vaporized and mixed with the process gas of the first oxidation stage in which methacrolein is prepared in gaseous form in a vaporizing plant in the presence of various gases and steam. In this way, recycled methacrolein can be resupplied to the process and the catalytic portion to be oxidized.

Description

technical field [0001] The present invention describes an improved process for the preparation of methacrylates, especially methacrylic acid and methyl methacrylate (MMA), based on C-4 starting materials. The C4 feedstock in this case is especially isobutene or tert-butanol. In addition, a wide range of embodiments for the efficient preparation of these products are provided. [0002] In particular, the invention relates to a process for the preparation of methacrylic acid and methyl methacrylate by gas-phase oxidation of isobutene. In the second gas-phase oxidation step, methacrolein is converted into methacrylic acid and unconverted methacrolein is removed from the methacrylic acid. This methacrolein is evaporated in an evaporation plant in the presence of various gases and vapours, and mixed in gaseous form with the process gas of the first oxidation stage in which methacrolein was produced. In this way, recycled methacrolein can be fed back to the process and catalytic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/055C07C51/25C07C67/08C07C69/54C07C45/35C07C47/22C07C1/24C07C11/09
CPCC07C51/252C07C67/08C07C45/35C07C1/24C07C57/04C07C69/54C07C47/22C07C11/09C07C51/25C07C67/44C07C67/48
Inventor S·科里尔G·科尔布尔J·邓
Owner ROHM G M B H
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