Catalyst for synthesizing methyl formate by formylating methyl nitrite, preparation method and application of catalyst

Abstract

The invention discloses a supported catalyst applicable to reaction for synthesizing methyl formate by formylating methyl nitrite. The supported catalyst comprises a palladium cyanide active component, a carrier and an optional accessory ingredient. According to the mass of the carrier, the percentage of the active component palladium cyanide is 0.01-2%, and the percentage of the accessory ingredient is less than or equal to 20%. The invention also discloses a preparation method of the catalyst applicable to reaction for synthesizing methyl formate by formylating methyl nitrite. The preparation method comprises the following steps: optionally dipping the carrier into water or ethanol solution of an accessory ingredient precursor, standing, drying and roasting; then dipping the carrier into water or ethanol solution of a palladium precursor, evenly stirring and evenly dispersing the carrier in a palladium precursor solution; carrying out ultrasound treatment under the heating condition until a solvent of the solution is volatilized to be dry, and evenly absorbing the palladium precursor on the surface of the carrier; drying and roasting an obtained absorption sample; and then reducing in the atmosphere of high-purity hydrogen to obtain a supported type palladium cyanide catalyst.

Description

technical field [0001] The invention belongs to the technical field of methyl formate synthesis, and relates to a catalyst for synthesizing methyl formate by formylation of methyl nitrite, a preparation method and an application thereof. Background technique [0002] Methyl formate is an extremely important intermediate in C1 chemistry and has a wide range of uses. Starting from methyl formate, formic acid, formamide, N,N-dimethylformamide, dimethyl carbonate, ethylene glycol, acetic acid, methyl acetate, acetic anhydride, methyl methacrylate, high-purity CO can be produced It can also be used as insecticide, fungicide, fumigant and tobacco treatment agent. At present, my country's annual demand for methyl formate is about 1.36 million tons, but the production capacity is about 50,000 tons, with a gap of 1.3 million tons. The consumption composition of methyl formate is as follows: 30% for synthetic leather, 26% for pesticide, 25% for medicine, 10% for acrylonitrile and 9%...

AI Technical Summary

Problems solved by technology

But adopt sodium methylate catalyst to have following serious shortcoming: (1) sodium methylate is extremely sensitive to water, thereby extremely high to the high purity requirement of raw material, wherein H 2 O.CO 2 , O 2 The content of impurities such as sulfide and sulfide should be less than 10 -6 , the water content in methanol should also be less than 10 -6 , the investment in high-purification equipment for raw materials is very high; (2) sodium methoxide is a strong base, which severely corrodes the equipment, and the reactor needs to be lined with titanium alloy, which is expensive; (3) it is carried out in a reactor, which is a homogeneous reaction , the separation of the catalyst and the product is troublesome, and a continuous production process cannot be realized; (4) the reaction pressure is relatively high, about 4MPa (40 atmospheric pressure), which belongs to a high-pressure reaction vessel; (5) the solubility of sodium methylate in methyl formate is small, if When the conversion rate of methanol is greater than a certain limit value, sodium methoxide will form solid precipitates, which will block the pipes and valves, which will bring great difficulties to the actual operation, and even fail to produce normally.

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