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Catalyst for catalytically synthesizing methyl formate under normal pressure and gas phase and preparation method thereof

A methyl formate and catalyst technology, which is applied in the field of methyl formate preparation, can solve the problems of severe equipment corrosion, high pressure requirements, and backward technology, and achieve the effects of reducing the average dispersed particle size, mild reaction conditions, and good catalytic activity

Inactive Publication Date: 2017-09-26
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the formic acid methanol esterification method has been gradually eliminated due to its backward technology, high energy consumption and serious equipment corrosion.
The liquid-phase methanol carbonylation method is currently the main method for producing methyl formate abroad. Its advantage is that the purity of the carbon monoxide feed gas is not high and the selectivity of the product methyl formate is high. However, this method also has serious disadvantages: sodium methoxide is The only catalyst, which requires anhydrous conditions; the reaction needs to be carried out in a reactor, and the pressure requirement is high; the separation of the product and the catalyst is troublesome; the process of methyl formate cannot be continuously produced, etc.
In view of the defects of the existing methyl formate production process and the serious shortage of domestic production capacity of methyl formate, it is necessary to develop a new catalyst with high activity and high selectivity for the formylation of methyl nitrite to synthesize methyl formate reaction

Method used

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  • Catalyst for catalytically synthesizing methyl formate under normal pressure and gas phase and preparation method thereof
  • Catalyst for catalytically synthesizing methyl formate under normal pressure and gas phase and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Dissolve 0.04mol of tetraethyl orthosilicate in 60mL of 6mol / L acetic acid solution, then add 0.04mol of zinc nitrate, 20mL of ethanol, 0.012g of palladium nitrate and 0.06g of PVP in sequence, keep stirring at room temperature for 2 hours, and dissolve them Transfer to a round-bottomed flask and use a rotary evaporator for vacuum distillation. After the solution evaporates, a transparent sol is obtained. Dry the sol in an oven at 100°C for 12 hours, and roast it in a muffle furnace at 450°C for 4 hours. The desired catalyst sample was obtained after reduction under a hydrogen atmosphere at °C for 2 hours, wherein the loading amount of the active component Pd was 0.1% of the weight of the carrier.

[0019] The phase structure analysis is carried out to the catalyst sample obtained in embodiment 1 by powder diffraction, the results are shown in figure 1 . Depend on figure 1 It can be seen that only SiO appears in the powder diffraction pattern 2 and the diffraction pe...

Embodiment 2

[0021] Dissolve 0.04mol of tetraethyl orthosilicate in 40mL of 6mol / L acetic acid solution, then add 0.06mol of zinc nitrate, 20mL of ethanol, 0.031g of palladium acetate and 0.31g of PVP in sequence, keep stirring at room temperature for 4 hours, and dissolve them Transfer to a round-bottom flask and use a rotary evaporator for vacuum distillation. After the solution evaporates, a transparent sol is obtained. Dry the sol in an oven at 110°C for 12 hours, and roast it in a muffle furnace at 500°C for 2 hours. The required catalyst sample was obtained by reduction under hydrogen atmosphere at °C for 4 hours, wherein the loading amount of the active component Pd was 0.2% of the mass of the carrier. The SiO in the catalyst sample was measured 2 The mass fraction of ZnO is 33.08%, and the mass fraction of ZnO is 57.87%.

Embodiment 3

[0023] Dissolve 0.04mol tetraethyl orthosilicate in 60mL acetic acid solution with a concentration of 6mol / L, then add 0.05mol zinc nitrate, 20mL ethanol, 0.054g tetraammine palladium nitrate and 0.324g PVP in sequence, and keep stirring at room temperature for 6h Then transfer it to a round-bottomed flask and use a rotary evaporator for vacuum distillation. After the solution evaporates, a transparent sol is obtained. Dry the sol in an oven at 80°C for 12 hours, and roast the solid in a muffle furnace at 600°C for 4 hours. The desired catalyst sample was obtained by reducing the substance under a carbon monoxide atmosphere at 200° C. for 2 hours, wherein the loading amount of the active component Pd was 0.3% of the weight of the carrier. The inductive plasma coupling test showed that the SiO in the catalyst sample 2 The mass fraction of ZnO is 37.05%, and the mass fraction of ZnO is 62.61%.

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Abstract

The invention discloses a catalyst for catalytically synthesizing methyl formate under normal pressure and a gas phase and a preparation method thereof. The preparation method of the catalyst comprises the following steps: adding tetraethyl orthosilicate, zinc nitrate, a precursor of an active component palladium, polyvinylpyrrolidone and ethanol into an acetic acid solution; after stirring and dissolving, carrying out decompression and distillation through a rotary evaporator to obtain transparent sol; drying the sol and roasting to obtain a precursor of the catalyst; reducing the precursor through hydrogen gas or carbon monoxide gas to obtain the catalyst Pd / (SiO2 and ZnO). The catalyst takes the palladium as the active component and SiO2 and ZnO composite oxide as a carrier. The catalyst disclosed by the invention has relatively good catalytic activity and methyl formate selectivity in reaction for synthesizing methyl formate under the normal pressure and the gas phase. According to the preparation method disclosed by the invention, the dispersion degree of the noble metal palladium in the carrier can be effectively improved through a sol-gel method and the catalytic efficiency of catalytic reaction is remarkably improved, so that efficient utilization of the noble metal palladium is realized.

Description

technical field [0001] The invention provides a catalyst for catalytically synthesizing methyl formate in an atmospheric pressure gas phase and a sol-gel preparation method thereof, which belong to the technical field of methyl formate preparation. Background technique [0002] Methyl formate is an important C1 chemical intermediate with a wide range of uses. In the chemical industry, it can be used as a raw material for organic synthesis products and as a solvent in the manufacture of cellulose acetate. In agriculture, it can be used as insecticide, cereal crop fungicide, fumigant and tobacco treatment agent, etc. In medicine, it is often used as a raw material for the synthesis of sulfomethylpyrimidine, sulfomethoxypyrimidine, and the antitussive agent methorphan. [0003] There are many methods for the preparation of methyl formate, the common ones are: formic acid methanol esterification method, methanol gas phase catalytic dehydrogenation method, formaldehyde catalyti...

Claims

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Application Information

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IPC IPC(8): B01J23/60B01J37/03B01J35/10C07C67/36C07C69/06
CPCC07C67/36B01J23/002B01J23/60B01J37/036B01J35/613B01J35/647C07C69/06
Inventor 姚元根张鑫潘鹏斌
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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