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Catalyst for synthesizing methyl formate by virtue of gas-phase methanol carbonylation as well as preparation method and application of catalyst

A gas-phase methanol, methyl formate technology, applied in the direction of carbon monoxide or formate reaction preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the difficult separation of catalyst and product, practical Difficulty in operation, inability to produce normally, etc., to achieve the effect of low impurity content, high selectivity and easy separation

Active Publication Date: 2014-04-02
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

But adopt sodium methylate catalyst to have following serious shortcoming: (1) sodium methylate is extremely sensitive to water, thereby extremely high to the 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 (2) Sodium methoxide is a strong base, which severely corrodes the equipment; (3) It is carried out in a reactor, which belongs to a homogeneous reaction, and it is difficult to separate the catalyst from the product; (4) The reaction pressure is relatively high, about 4MPa; (5) Methanol The solubility of sodium in methyl formate is small. If the conversion rate of methanol is greater than a certain limit value, sodium methoxide will form a solid precipitate, which will block the pipeline and valve, which will bring great difficulties to the actual operation and even fail to produce normally.

Method used

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  • Catalyst for synthesizing methyl formate by virtue of gas-phase methanol carbonylation as well as preparation method and application of catalyst
  • Catalyst for synthesizing methyl formate by virtue of gas-phase methanol carbonylation as well as preparation method and application of catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 1g of alumina and impregnate it into 15mL of 50mmol / L CuCl 2 2H 2 O ethanol solution, let it stand for 18 hours, dry at 100°C for 15 hours, roast at 400°C for 5 hours, then re-immerse in 1.25mL of 37.6mmol / L potassium chloropalladate aqueous solution, then add 4mL of water, stir for 3 hours, Ultrasonic dispersion for 3 hours, drying at 120°C for 15 hours, roasting at 400°C for 5 hours, adding 0.1g ascorbic acid, 0.2g citric acid, 0.5g polyvinylpyrrolidone, reducing at 90°C for 1 hour, and drying at 60°C for 15 hours in a vacuum. Pd-Cu / Al in the Gas-Phase Methanol Carbonylation to Methyl Formate 2 o 3 Catalyst 1.

Embodiment 2

[0032] Weigh 1g of alumina and impregnate it into 15mL of 50mmol / L CuCl 2 2H 2 O ethanol solution, let it stand for 18 hours, dry at 100°C for 15 hours, bake at 400°C for 5 hours, then re-immerse in 0.68mL of 37.6mmol / L aqueous solution of chloroplatinic acid, add 4mL of water, stir for 3 hours, and ultrasonically disperse For 3 hours, dry at 120°C for 15 hours, roast at 400°C for 5 hours, add 0.1g ascorbic acid, 0.2g citric acid, 0.5g polyvinylpyrrolidone, reduce at 90°C for 1 hour, and dry at 60°C for 15 hours in a vacuum, then it will be used in gas phase methanol Pt-Cu / Al in Carbonylation Synthesis of Methyl Formate2 o 3 Catalyst 2.

Embodiment 3

[0034] Weigh 1g of Ni(NO) of magnesia 17mL50mmol / L 3 ) 2 ·6H 2 In O ethanol solution, let stand for 18 hours, dry at 100°C for 15 hours, roast at 400°C for 5 hours, then re-impregnate into 0.63mL37.6mmol / L of potassium chloropalladate and 0.34mL37.6mmol / L of chloroplatinic acid Add 4mL of water to the aqueous solution, stir for 3 hours, ultrasonically disperse for 3 hours, dry at 120°C for 15 hours, bake at 400°C for 5 hours, add 1mL of formaldehyde, 0.24g of sodium citrate, 0.6g of polyethylene oxide-polyepoxide Propane-polyethylene oxide triblock copolymer was reduced at 100°C for 2 hours and dried at 60°C in vacuum for 15 hours to obtain PtPd-Ni / MgO catalyst 3 for the gas-phase methanol carbonylation to methyl formate reaction.

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Abstract

The invention discloses a supported nano platinum group metal heterogeneous catalyst for synthesizing methyl formate by virtue of gas-phase methanol carbonylation. The supported nano platinum group metal heterogeneous catalyst is prepared from the following components accounting for the mass of a carrier: 0.01-2 percent of platinum group metal active component, and smaller than or equal to 20% of an optional additive. The invention also discloses a preparation method of the supported nano platinum group metal heterogeneous catalyst for synthesizing the methyl formate by virtue of the gas-phase methanol carbonylation. The preparation method comprises the following steps: optionally immersing the carrier into an aqueous or ethanol solution of an additive precursor, standing, drying, and roasting; then immersing the carrier into an aqueous or ethanol solution of a platinum group metal precursor, and uniformly mixing to enable the carrier to be uniformly dispersed in the platinum group metal precursor solution; carrying out ultrasonic waves treatment under the heating condition until a solvent of the solution volatilizes to be dry, and enabling the platinum group metal precursor to be uniformly adsorbed on the surface of the carrier; drying and roasting an obtained adsorbed sample; then adding a reducing agent, a structure-directing agent and a protective agent to carry out reduction reaction; and then carrying out filtering, washing and vacuum drying to obtain the supported nano platinum group metal heterogeneous catalyst.

Description

technical field [0001] The invention belongs to the technical field of methyl formate synthesis, and relates to a supported nanometer platinum group metal heterogeneous catalyst for synthesizing methyl formate by vapor-phase methanol carbonylation and a preparation method thereof. Background technique [0002] Methyl formate is a very important intermediate in carbon-chemistry and has a wide range of uses. From methyl formate, formic acid, formamide, N,N-dimethylformamide, dimethyl carbonate, ethylene glycol, acetic acid, methyl acetate, acetic anhydride, methyl methacrylate, high-purity Products such as CO and diphosgene can also be used as insecticides, fungicides, fumigants and tobacco treatment agents. At present, the annual production capacity of methyl formate in my country is about 50,000 tons, and the demand is about 100,000 tons. The consumption structure is as follows: synthetic leather accounts for 30%, pesticides account for 26%, medicine accounts for 25%, acryl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/44C07C67/36C07C69/06
Inventor 徐忠宁郭国聪彭思艳王志巧陈青松王明盛姚元根
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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