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Catalyst for preparing methyl nitrite by reducing dilute nitric acid through methanol and preparation thereof

A technology of methyl nitrite and catalyst, which is applied in the direction of nitrite preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., to achieve the effect of high strength and high activity

Active Publication Date: 2015-09-30
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

There are few reported processes on the catalytic system of methanol reduction of dilute nitric acid to prepare methyl nitrite, which can be said to be blank in this field

Method used

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  • Catalyst for preparing methyl nitrite by reducing dilute nitric acid through methanol and preparation thereof
  • Catalyst for preparing methyl nitrite by reducing dilute nitric acid through methanol and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1g of SiO with a particle size of 5 mesh 2 The pellets were dispersed in 10ml of 15wt% glucose aqueous solution, added with 0.6g of concentrated sulfuric acid, left at room temperature for 12h, then dried under vacuum at 50°C for 2h; 2 Under the atmosphere, the temperature is programmed from room temperature to the calcination temperature, and the calcination is carbonized. The temperature programming rate is 1°C / min, the calcination temperature is 600°C, and the calcination time is 1h, and the carbon-coated SiO is obtained. 2 Pellets, named SiO 2 5gC-15wt%.

[0017] Subsequently, 1 g of the obtained carbon-coated SiO 2 Pellet SiO 2 5gC-15wt%, dispersed in 10ml containing 0.16g ZrOCI 2 ·8H 2 In aqueous solution of O, place at room temperature for 12h, then in N 2 Under the atmosphere, the temperature was programmed from room temperature to the roasting temperature, roasted and carbonized, the programmed temperature increase rate was 1°C / min, the roasting temperatu...

Embodiment 2

[0019] The preparation method and steps of catalyst B-W are the same as those of catalyst A, the difference is the type and size of carrier pellets, the type and concentration of carbon deposition precursor, calcination temperature and time; the type and quantity of metal precursor, calcination temperature, etc., the obtained catalyst named MO x -a wt% / SbgC-c wt%-d-e or MO x -a wt% / SbsC-cwt%-d-e. where MO x Represents the type of metal oxide; a represents the loading capacity of metal oxide; S represents the type of carrier; b represents the mesh number of the carrier; c represents the concentration of carbon deposition precursor; d represents the calcination temperature; e represents the calcination temperature; g represents the carbon deposition precursor is glucose; s means that the carbon deposition precursor is sucrose. See Table 1 for details.

[0020] Table 1 Catalyst B-W preparation conditions

[0021]

[0022]

Embodiment 3

[0024] The obtained catalysts A-J are used for methanol reduction of dilute nitric acid to prepare methyl nitrite. The reaction is carried out on a fixed-bed reaction device. Catalysts A-J are added to a glass tube reactor, and the upper part of the catalyst is filled with silica pellets (preheated raw materials ), the lower part is filled with stainless steel wire (supporting the catalyst layer). Under a hydrogen atmosphere, the catalyst was reduced at 400°C for 5 hours; under a nitrogen atmosphere, the reaction device was heated to a certain temperature, and 2wt% dilute nitric acid and 18wt% methanol aqueous solution were added with a metering pump. The reaction temperature is 70°C and the WHSV is 2.5h -1 , the pressure is normal pressure. The content of nitric acid in the effluent was analyzed by ionic liquid chromatography, and the conversion rate of nitric acid was calculated; the content of methyl nitrite in the gas was analyzed by gas chromatography, and the selectivit...

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Abstract

The invention discloses a catalyst for preparing methyl nitrite by reducing dilute nitric acid through methanol and preparation thereof. The catalyst is characterized in that SiO2 and Al2O3 pellets with the particle sizes being 5-20 meshes are adopted as carriers, transition metal oxides with oxidation reduction are taken as active components, carbon deposits are taken as auxiliary active components, the active components are highly dispersed on the carriers, the content range is 0.5-5wt%, and the carriers are wrapped by the auxiliary active components. The transition metal oxides with oxidation reduction are one or two of Mn3O4, CeO2, ZrO2, Co3O4, MoO3 and V2O5. The precursors of the carbon deposits are one of glucose and saccharose. According to the catalyst, the carriers have the advantages of high strength and wear resistance; an auxiliary catalyst has the advantage of high specific surface, the active components can be highly dispersed on the carriers due to the assistance of the auxiliary catalyst, so that the high activity is shown in the process of preparing methyl nitrite by reducing dilute nitric acid through methanol.

Description

technical field [0001] The invention belongs to the field of coal chemical catalysis, and specifically reduces the dilute nitric acid waste liquid produced in the coal chemical process to nitrous acid, and the nitrous acid reacts with methanol in the system to form methyl nitrite, which is the catalyst for the production of ethyl nitrite from coal. An important intermediate in the diol process, thereby reducing waste liquid discharge. Background technique [0002] It is of great significance to efficiently convert my country's abundant coal reserves into ethylene glycol, a basic chemical raw material, and reduce the dependence of chemical raw materials on relatively poor petroleum resources, which is conducive to the optimization of my country's energy and resource structure. [0003] At present, the coal-to-ethylene glycol process is mainly divided into five modules, namely raw material gas preparation tower, esterification tower, oxidative carbonylation tower, hydrogenatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/08B01J23/34B01J23/10B01J23/75B01J23/28B01J23/22C07C203/00C07C201/04
Inventor 马继平徐杰高进郑玺贾秀全王敏苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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