A kind of method for preparing methyl nitrite from nitric acid

A technology of methyl nitrite and nitric acid, applied in the direction of nitrite preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of dilute nitric acid pollution, large environmental impact, difficult to handle, etc. Good stability, high activity and selectivity, the effect of solving dilute nitric acid pollution and waste of resources

Active Publication Date: 2022-08-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the current coal-to-ethylene glycol process, a large amount of dilute nitric acid waste liquid is produced, it is difficult to handle, the environmental impact is large, and the existing reported catalyst strength and stability and activity and selectivity need to be further improved. The purpose of the invention is to : To develop a method for preparing methyl nitrite with dilute nitric acid, which has the advantages of good catalyst strength and stability, high activity and selectivity, and can be applied to the process of coal-to-ethylene glycol, which can solve the problems of dilute nitric acid pollution and waste of resources.

Method used

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  • A kind of method for preparing methyl nitrite from nitric acid
  • A kind of method for preparing methyl nitrite from nitric acid
  • A kind of method for preparing methyl nitrite from nitric acid

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 50g of 10-20 mesh silica, 0.2g of vinylpyrrolidone-vinyl acetate copolymer, and 100g of ethyl acetate into a 250ml reaction flask, keep a constant temperature water bath at 70°C, stir mechanically, add 10g of vinylpyrrolidone and 75mg of an initiator coupler. Nitrogen bisisobutyronitrile was reacted under nitrogen protection for 6 hours, cooled to room temperature and filtered. The obtained solid was dried at 100 °C for 24 hours and then passed through a 10-20 mesh sieve to obtain 59 g of a nitrogen-containing organic polymer-coated silicon-containing inorganic compound, namely a polymer Vinylpyrrolidone-coated silica, denoted as PVP@SiO 2 .

[0027] Take 5g PVP@SiO 2 , add 5ml of ruthenium trichloride aqueous solution prepared with 0.5g of hydrated ruthenium trichloride, stir evenly, let stand for 24h, dry at 100°C for 12h, N 2 It was calcined at 450 °C for 3 h under the protection to obtain a core-shell catalyst, that is, a nitrogen-doped carbon-coated core-shel...

Embodiment 2～6

[0030] The specific practices of Examples 2 to 6 are similar to those of Example 1, except that the prepared nitrogen-doped carbon-coated core-shell supported metal catalysts have silicon dioxide or silicon carbide as the core and ruthenium or gold as the metal.

Embodiment 2

[0032] The difference from Example 1 is that 50 g of 10-20 mesh silicon carbide, 0.2 g of vinylpyrrolidone-vinyl acetate copolymer, and 100 g of ethyl acetate were added to a 250 ml reaction flask. Finally, a nitrogen-doped carbon-coated core-shell silicon carbide-supported ruthenium catalyst was obtained, denoted as Ru-N-C@SiC.

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Abstract

The present application discloses a method for preparing methyl nitrite with dilute nitric acid. The method comprises: in a fixed bed reactor, contacting raw materials containing nitric acid and methanol with a catalyst to react to obtain methyl nitrite. Wherein, the catalyst has a core-shell structure; the inner core of the catalyst includes a silicon-containing inorganic compound; the silicon-containing inorganic compound includes at least one of silicon dioxide and silicon carbide; the outer shell of the catalyst includes nitrogen-doped carbon ; Metal elements are loaded on the nitrogen-doped carbon; the metal elements are selected from at least one of ruthenium and gold. When dilute nitric acid and methanol are reacted to prepare methyl nitrite, using the catalyst, the conversion rate of nitric acid and the selectivity of methyl nitrite can reach over 99% at the highest.

Description

technical field [0001] The application relates to a method for preparing methyl nitrite from nitric acid, and belongs to the technical field of organic chemical industry. Background technique [0002] Ethylene glycol is an important bulk chemical, mainly used in the production of polyester materials such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), as well as antifreeze and moisture absorbent and organic solvents. my country's ethylene glycol consumption exceeds 12 million tons per year, and the import dependence is as high as 60%. The traditional production method of ethylene glycol adopts the petrochemical route, which is obtained from ethylene through epoxidation, hydration and other processes. my country's oil resources have long been dependent on imports. In 2017, my country's apparent oil consumption was 590 million tons and imports were 396 million tons, with an import dependence of 67%. In view of the current situation of my country's "...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/04C07C203/00B01J27/24
CPCC07C201/04B01J27/24C07C203/00
Inventor 黄义争高进徐杰孙颖苗虹马红马继平车鹏华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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