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Methyl methoxyacetate production method

A technology of methyl methoxyacetate and carbon monoxide is applied in the synthesis field of methyl methoxyacetate to achieve the effects of easy preparation, mild reaction conditions and reduced operating costs

Inactive Publication Date: 2016-04-13
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

However, at present, industrial methanol oxidation needs to be carried out at high temperature (300-400°C), while carbonylation reaction is carried out at a lower reaction temperature, so the methanol industrial oxidation catalyst and carbonylation catalyst are only packed in the same It is impossible to directly prepare methyl methoxyacetate from methanol in the reactor

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The preparation of embodiment 1 oxidation catalyst

[0045] Preparation of oxidation catalyst: Pour 4.76g of oxalic acid into 30ml of deionized water, stir to obtain an oxalic acid solution, add 2.22g of ammonium metavanadate to the oxalic acid solution, stir to obtain a dark green solution, add 10g of titanium dioxide powder, and stir evenly to obtain a paste After standing for 4 hours, it was dried in an oven at 100° C. for 12 hours, and then fired in a muffle furnace at 400° C. for 4 hours to obtain an oxidation catalyst precursor. Dissolve 0.25g of titanium sulfate in 6ml of deionized water, take 5g of oxidation catalyst precursor powder and immerse in the titanium sulfate solution, immerse at room temperature for 12h, dry at room temperature, dry at 100°C, and then bake in a muffle furnace at 400°C 4h. Press the calcined powder into tablets, crush it, and sieve the 40-60 mesh particles to obtain the oxidation catalyst, which is denoted as O1 # .

[0046] O2 # ~...

Embodiment 2

[0049] Embodiment 2 Oxidation catalyst composition analysis

[0050] Oxidation catalyst O1 was analyzed by X-ray fluorescence spectrometry #~O6 # The composition was analyzed, and the results are shown in Table 2.

[0051] Table 2

[0052]

Embodiment 3

[0053] Embodiment 3 solid acid catalyst

[0054] The relationship between the solid acid catalyst sample number and the catalyst type is shown in Table 3.

[0055] Among them, A1 # The perfluorosulfonic acid resin (NafionNR50) was purchased from Sigma-Aldrich, and was dried at 105°C for 12 hours in an air atmosphere before use, and 40-60 mesh particles were sieved.

[0056] A2 # ~A4 # Hydrogen-type molecular sieves were purchased from Nankai University Catalyst Factory. After roasting, tableting, crushing, and 40-60 mesh particles are sieved for later use.

[0057] A5 # 、A6 # Purchased from Sinopharm Chemical Reagent Co., Ltd., and dried in air at 100°C for 2 hours before use.

[0058] table 3

[0059] serial number

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Abstract

The invention relates to a methyl methoxyacetate production method, which comprises that methanol is sequentially subjected to methanol oxidation to generate formaldehyde, methanol and formaldehyde condensation reaction to synthesize methylal, and methylal carbonylation reaction to generate methyl methoxyacetate on an oxidation catalyst and a solid acid catalyst in a reactor. According to the method of the present invention, the three steps of the reactions are integrated into the one reactor, such that the process can be simplified, the investment can be saved, the operation cost can be reduced, and the effective way can be provided for the synthesis of the methyl methoxyacetate.

Description

technical field [0001] The application relates to a synthetic method of methyl methoxyacetate. Background technique [0002] Methyl methoxyacetate is an important organic chemical raw material that can be used to prepare a variety of chemical products. One of the very important downstream products is ethylene glycol, which is an important monomer for the synthesis of polyester fibers. In addition, it is an important antifreeze. At present, the production route of ethylene glycol mainly relies on olefins obtained from petrochemical industry. Due to the shortage and non-renewability of petroleum resources, it is necessary to develop non-petroleum routes to produce ethylene glycol. [0003] Methanol can currently be obtained through the coal chemical industry route. If methanol can be directly oxidized and carbonylated to produce methyl methoxyacetate, it will have significant advantages such as less investment, low operating and production costs. However, at present, indust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/36
Inventor 刘世平朱文良刘红超刘勇倪友明刘中民李利娜周慧
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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