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Process for purifying methyl methacrylate to remove low boiling components

A technology of alkyl methacrylate and methacrolein, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., and can solve problems such as expensive variants

Pending Publication Date: 2022-05-06
罗姆化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method variant - especially with regard to energy requirements and the required number of separation devices - is very expensive

Method used

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  • Process for purifying methyl methacrylate to remove low boiling components
  • Process for purifying methyl methacrylate to remove low boiling components

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] stay Figure 1 In the continuous operation equipment shown in, the distillate stream (31) of the high boiling tower (Distillation Tower IV) (26) is generated and purified by distillation in the subsequent low boiling tower (distillation tower I) (32) to remove the low boiling. With this operation, MMA bottom stream containing process stabilizer can be generated, which has PRAME content of < 10 ppm and ibsme content of < 350 ppm.

[0046] The low boiling tower is operated at an absolute operating pressure of 250 mbar. The tower is equipped with structured packing M750 from Sulzer Y (diameter 100mm, filling height 12000mm, feeding at 6000mm). Add the process stabilizer to the condenser. The process stabilizer is dissolved in MMA and added at a rate of 330g / h. The temperature is controlled at an operating temperature of 20 ° C and a phase separator with water feeding (34) produces an aqueous phase (36) and an organic phase. The organic phase is recirculated into the tower as ...

Embodiment 2

[0049] Using the tower (250 mbar absolute operating pressure) and phase separator (operating temperature 20 ℃) of example 1, the distillate stream (31) (11000g / h) of the high boiling tower is distilled, including 96.7 wt% MMA and 1.8 wt% H 2 O. 0.1 wt% mal, 0.1 wt% PRAME, 0.2 wt% ibsme and 1.1 wt% residue). Here, the ratio of reflux to feed is set to 2.2 and the discharge stream is fixed at 25 g / h. The water addition rate in the phase separator is 1530 g / h. This results in a top temperature of 54 ° C and a bottom temperature of 62 ° C. The aqueous stream (36) of the phase separator is 1858 g / h and contains 1.6% by weight of MMA and 91.8% by weight of H 2 O. 0.4 wt% mal, 0.4 wt% PRAME, 0.5 wt% ibsme and 4.9 wt% residue. The bottom output (40) is 11035g / h, which consists of 99.91 wt% MMA, 35ppm PRAME, 315ppm ibsme and 0.06 wt% process stabilizer. This mode of operation described achieves an MMA retention rate of 99.71%.

Embodiment 3

[0051] In the tower (250 mbar absolute operating pressure) and phase separator (operating temperature 20 ℃) of embodiment 1, the distillate stream (31) (11000g / h) of the distillation high boiling tower contains 96.7 wt% MMA and 1.8 wt% H 2 O. 0.1 wt% mal, 0.1 wt% PRAME, 0.2 wt% ibsme and 1.1 wt% residue). Here, the ratio of reflux to feed is set to 2.0 and the discharge flow is fixed at 25 g / h. No water is added to the phase separator. This results in a top temperature of 50 ° C and a bottom temperature of 62 ° C. The aqueous stream (36) of the phase separator is 335g / h and contains 5.5% by weight of MMA and 60.0% by weight of H 2 O. 2.0 wt% mal, 1.5 wt% PRAME, 2.0 wt% ibsme and 29.0 wt% residue. The bottom output (40) is 11000 g / h, which consists of 99.9 wt% MMA, 55 ppm PRAME, 320 ppm ibsme and 0.06 wt% process stabilizer. The MMA retention rate of 99.51% is achieved.

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Abstract

The present invention relates to a novel process for purifying methyl methacrylate contaminated with low boiling components by distillation, wherein the MMA is prepared by oxidative esterification and contains methyl propionate (PRAME), methyl isobutyrate (IBSME) and methylacrolein (MAL) as low boiling components as crude products. In this case, the method can be applied to MMA produced from C2-based methacrolein, which contains the indicated low-boiling components. However, the process is also theoretically transferable to MMA prepared from C4-based methacrolein, which contains PRAME and MAL but does not have a significant amount of IBSME.

Description

technical field [0001] The invention relates to a new method for purifying methyl methacrylate (MMA) contaminated by low boiling components by distillation, wherein the MMA is prepared by oxidative esterification and contains methyl propionate (PRAME), methyl isobutyrate (ibsme) and methylacrolein (mal) as low boiling components as crude products. Here, the method can be applied to MMA prepared from C2 based methylacrolein, which contains the specified low boiling point component. However, the method can theoretically also be transferred to MMA prepared from C4 based methylacrolein, which contains PRAME and mal but no significant amount of ibsme. Background technology [0002] At present, methyl methacrylate (MMA) is obtained from C 2 -、C 3 -Or C 4 -The synthesis unit is prepared by various methods. In one of these methods, MMA is obtained by direct oxidative esterification of methylacrolein with methanol. Here, methacrolein is obtained from propionaldehyde and formaldehyde in th...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/39C07C67/54C07C67/60C07C67/48C07C69/24
CPCC07C67/39C07C67/54C07C67/60C07C67/48C07C67/58C07C45/75C07C69/54C07C47/22C07C69/24C07C67/44C07C67/62B01D3/14
Inventor S·克里尔D·H·科尼格B·艾特艾萨
Owner 罗姆化学有限责任公司
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