Methyl methoxyacetate (MMAC) synthesis method

A technology of methyl methoxyacetate, chemical synthesis, applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, molecular sieve catalysts, etc., can solve problems such as high reactivity

Inactive Publication Date: 2014-10-29
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

The process adopts a gas-solid phase fixed bed catalytic reaction process, and the reaction pressure is lower than 1MPa, which overcomes the need for high CO pressu

Method used

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  • Methyl methoxyacetate (MMAC) synthesis method
  • Methyl methoxyacetate (MMAC) synthesis method
  • Methyl methoxyacetate (MMAC) synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Hydrogen type MCM-22 molecular sieve (SiO 2 / Al 2 o 3Ratio 45) 50 mg, placed in a tubular stainless steel fixed-bed reactor, heated from room temperature to 500 °C at 5 °C / min in 50 ml / min He, cooled to 90 °C after 500 °C treatment for 1 hour, and introduced CO and DMM mixed gas, DMM partial pressure is 1.8kPa, CO partial pressure is 398.2kPa, and the space velocity under normal pressure is 300L·g -1 h -1 . The reaction tail gas was detected online by gas chromatography. The above process was repeated, and the reaction temperature was changed at 100°C, 110°C, 120°C, 130°C and 140°C, respectively.

Embodiment 2

[0036] Embodiment 2: Hydrogen type MCM-49 molecular sieve (SiO 2 / Al 2 o 3 Ratio 25) 50 mg, placed in a tubular stainless steel fixed-bed reactor, heated from room temperature to 500 °C at 5 °C / min in 50 ml / min He, cooled to 110 °C after 500 °C treatment for 1 hour, and introduced CO and DMM mixed gas, DMM partial pressure is 1.8kPa, CO partial pressure is 398.2kPa, and the space velocity under normal pressure is 300L·g -1 h -1 . The reaction tail gas was detected online by gas chromatography.

Embodiment 3

[0037] Embodiment 3: Hydrogen type Beta molecular sieve (SiO 2 / Al 2 o 3 Ratio 25) 50mg reaction performance test, the operation is the same as in Example 2.

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Abstract

The invention discloses a catalyst for synthesis of methyl methoxyacetate (MMAC) by use of dimethoxymethane (DMM) and CO as raw materials, the catalyst is a molecular sieve with twelve membered ring cavity, ten membered ring channel and supercage structures, the International Zeolite Association (IZA) defines the topological structure of the catalyst as MWW type such as MCM-22 and MCM-49, the molecular formula is SixAlyOz, and the molecular sieve is hydrogen type. The molecular sieve SiO2 / Al2O3 ratio is 10-200. Carbonylation reaction is performed in a gas-solid phase fixed bed reactor, the reaction pressure is 1-50*105Pa, a reaction raw material gas comprises the dimethoxymethane with the partial pressure of 1-50kPa and balance of CO (1-49*105Pa) or CO / He (1-49* 105Pa), the reaction temperature is 60-180 DEG C, and the space velocity is 20-500L .g<-1>.h<-1>. Compared with a MFI type molecular sieve (HZSM-5) only having a crossed ten membered ring structure and a BEA type molecular sieve (Hbeta) only having a twelve membered ring structure, the MWW type molecular sieve has higher methyl methoxyacetate selectivity.

Description

technical field [0001] The invention relates to a catalyst and application for synthesizing methyl methoxyacetate (MMAC) from methylal (DMM) and CO carbonylation. Specifically, the present invention provides a new catalyst for catalyzing methylal to synthesize methyl methoxyacetate through carbonylation reaction: MCM-22, MCM-49, or a mixture thereof, or a system made of loaded Pd, Cu, Rh, Ir, etc. prepared supported catalysts. Background technique [0002] Methyl methoxyacetate (MMAC) is a colorless transparent liquid with a boiling point of 129-130°C under normal pressure and a flash point of 35°C. It is slightly soluble in water. Methyl methoxyacetate is an important intermediate in the synthesis of medicines, and has important applications in the synthesis of vitamin B6, sulfonamide (sulfonamide-5,6-dimethoxine), etc. More importantly, ethylene glycol monomethyl ether can be obtained by hydrogenation reduction of methyl methoxyacetate, and ethylene glycol monomethyl eth...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/36B01J29/76B01J29/70
CPCB01J29/7038B01J29/7676B01J2229/18C07C67/36C07C69/708
Inventor 展恩胜申文杰黄秀敏薛会福
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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