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

A technology of methyl nitrite and methyl formate, applied in the direction of carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve practical operation difficulties and reaction pressure. high, equipment corrosion and other problems, to achieve the effect of low impurity content, high CO conversion rate and high selectivity

Active Publication Date: 2014-07-02
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
View PDF1 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 i

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Catalyst for synthesizing methyl formate by formylating methyl nitrite, preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 1g of magnesium oxide and impregnate it into 17mL of 50mmol / L Ni(NO 3 ) 2 ·6H 2 O ethanol solution, let it stand for 10 hours, dry at 120°C for 10 hours, roast at 500°C for 4 hours, then re-immerse in 1.25mL of 37.6mmol / L potassium chloropalladate aqueous solution, add 4mL of water, and stir for 4 hours. Ultrasonic dispersion for 4 hours, drying at 120°C for 10 hours, calcining at 500°C for 4 hours, and then reducing at 400°C for 5 hours under a high-purity hydrogen atmosphere to obtain PdH used in the formylation of methyl nitrite to methyl formate x - Ni / MgO Catalyst 1 .

Embodiment 2

[0023] Weigh 1g of alumina and impregnate it into 1.25mL of 37.6mmol / L potassium chloropalladate aqueous solution, add 4mL of water, stir for 4 hours, ultrasonically disperse for 4 hours, dry at 120°C for 10 hours, bake at 500°C for 4 hours, and then Reduction at 400°C for 5 hours under a high-purity hydrogen atmosphere to obtain PdH used in the formylation of methyl nitrite to methyl formate x / A1 2 o 3 Catalyst 2.

Embodiment 3

[0025] The catalyst of embodiment 1-2 is applied in methyl nitrite formylation synthesis methyl formate reaction, feed gas ratio is methyl nitrite: carbon monoxide: hydrogen: nitrogen=20: 20: 10: 50 (volume ratio) , the gas phase space velocity is 3000h -1 , the reaction temperature is 120°C, the reaction pressure is 0.1MPa, and the reaction results are shown in Table 1.

[0026] The performance of table 1 embodiment catalyst in methyl nitrite formylation synthetic methyl formate reaction

[0027]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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%...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J31/26B01J31/12C07C69/06C07C67/36
Inventor 徐忠宁郭国聪彭思艳王志巧吕冬梅陈青松王明盛
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap