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Treatment method for by-products of methyl formate and methylal in production of dimethyl carbonate by carbonylation method

A technology of dimethyl carbonate and methyl formate, applied in the field of chemical technology, can solve problems such as not being retrieved, and achieve the effects of avoiding hydrogenation conversion, saving consumption, and low reaction temperature

Pending Publication Date: 2021-03-09
上海诺哈尔化工技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Treatment method for by-products of methyl formate and methylal in production of dimethyl carbonate by carbonylation method
  • Treatment method for by-products of methyl formate and methylal in production of dimethyl carbonate by carbonylation method

Examples

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Effect test

Embodiment 1

[0039] Pressurize 2000.0kg / h of material (the mass content is ME: 97.2%, MF: 0.4%, ML: 0.8%, DMC: 1.6%) to 3.0MPa(G), and the flow rate is 30.73NM 3Mix 3.0MPa(G) hydrogen per hour, heat to 95.0°C, and carry out hydrogenation reaction in the reactor. The hydrogenation catalyst is a nickel-based catalyst. The hourly space velocity is 3.0h -1 , The reacted material is cooled to 40.0°C by a circulating water cooler, and the gas-liquid separation is carried out in the flash tank, and the pressure of the flash tank is 0.5MPa(G). The vent gas is discharged from the top of the flash tank, and the pressure of the control tank is kept constant. The liquid at the bottom of the flash tank is the product after hydrogenation, which is sent to chromatographic analysis. It can be calculated that the conversion rate of MF is 72.3%, the conversion rate of ML is 81.2%, and the conversion rate of DMC is 18.1% %.

Embodiment 2

[0041] Pressurize the 2200.0kg / h material (the mass content is ME: 97.8%, MF: 0.7%, ML: 0.7%, DMC: 0.8%) to 4.0MPa (G), and the flow rate is 30.73NM3 / h 4.0MPa ( G) Hydrogen is mixed, heated to 135.0°C, and hydrogenation reaction is carried out in the reactor. The hydrogenation catalyst is a nickel-based catalyst, the reaction temperature is 140.0°C, the reaction temperature and pressure are 4.0MPa(G), and the liquid hourly space velocity is 2.0h -1 , The reacted material is cooled to 40.0°C by a circulating water cooler, and the gas-liquid separation is carried out in the flash tank, and the pressure of the flash tank is 0.5MPa(G). The vent gas is discharged from the top of the flash tank, and the pressure of the control tank is kept constant. The liquid at the bottom of the flash tank is the product after hydrogenation, which is sent to chromatographic analysis. It can be calculated that the conversion rate of MF is 80.2%, the conversion rate of ML is 88.5%, and the conversion...

Embodiment 3

[0043] Pressurize 2600.0kg / h of material (the mass content is ME: 95.0%, MF: 0.2%, ML: 0.8%, DMC: 4.0%) to 2.0MPa(G), and the flow rate is 40.27NM 3 Mix 2.0MPa(G) hydrogen per hour, heat to 115.0°C, and carry out hydrogenation reaction in the reactor. The hydrogenation catalyst is a palladium-based catalyst. The hourly space velocity is 5.0h -1 , The reacted material is cooled to 40.0°C by a circulating water cooler, and the gas-liquid separation is carried out in the flash tank, and the pressure of the flash tank is 0.5MPa(G). The vent gas is discharged from the top of the flash tank, and the pressure of the control tank is kept constant. The liquid at the bottom of the flash tank is the product after hydrogenation, which is sent to chromatographic analysis. It can be calculated that the conversion rate of MF is 82.3%, the conversion rate of ML is 90.4%, and the conversion rate of DMC is 10.5% %.

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Abstract

The invention discloses a treatment method for by-products of methyl formate and methylal in production of dimethyl carbonate by a carbonylation method, and relates to the field of chemical processes.The process flow comprises the following steps: materials of mixture of methanol, methyl formate, methylal, dimethyl carbonate and the like are pressurized by a pump and then mixed with high-pressurehydrogen of the materials to form materials, the materials are heated to the reaction temperature by a preheater, and the heated materials are sent into a reactor; a cooled material is fed into a low-pressure flash tank; and non-condensable gas methane, hydrogen and other materials are discharged from the tank top of the low-pressure flash tank, the materials obtained from the tank kettle of thelow-pressure flash tank are high-concentration methanol, the materials pressurized by the pump can be fed into a dimethyl carbonate reaction process to be recycled, and part of the materials can be subjected to cyclic hydrogenation. According to the invention, a mixture of methanol, methyl formate, methylal and dimethyl carbonate does not need to be gasified, and the reaction can be carried out under the working condition of a trickle bed, so that the consumption of steam and circulating water is reduced, the hydro-conversion efficiency of methyl formate and methylal is improved, and the hydro-conversion of dimethyl carbonate is avoided.

Description

technical field [0001] The invention belongs to the field of chemical technology, and relates to the hydrogenation treatment technology of methyl formate and methylal, in particular to the method for producing methanol through the hydrogenation reaction of methyl formate and methylal, the by-products of dimethyl carbonate produced by gas-phase carbonylation. Background technique [0002] The main raw materials for the production of dimethyl carbonate by gas-phase carbonylation are carbon monoxide (CO) and methanol, the main reaction product is dimethyl carbonate, and the by-products are methyl formate, methylal, dimethyl oxalate (DMO), etc. Since the boiling points of methyl formate and methylal are relatively close to those of methanol, and methylal and methanol azeotrope, methanol and dimethyl carbonate are azeotropic, so in the dimethyl carbonate rectification system and methanol dehydration recovery system, both There are a large amount of mixtures such as methyl formate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/132C07C29/149C07C29/80C07C31/04C07C68/00C07C69/96
CPCC07C29/132C07C29/149C07C29/80C07C68/00C07C31/04C07C69/96Y02P20/52
Inventor 汪俊肖招金单文波唐大川倪菁华
Owner 上海诺哈尔化工技术有限公司
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