Methyl nitrite preparation method by reaction of NO and nitric acid and methanol

A technology of methyl nitrite and methanol, applied in the preparation of nitrite, organic chemistry and other directions, can solve the problems of equipment corrosion and high nitrogen oxide supply cost, and achieve the effect of good technical effect

Active Publication Date: 2017-04-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of high nitrogen oxide supply cost and serious equipment corrosion existing in the

Method used

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  • Methyl nitrite preparation method by reaction of NO and nitric acid and methanol
  • Methyl nitrite preparation method by reaction of NO and nitric acid and methanol
  • Methyl nitrite preparation method by reaction of NO and nitric acid and methanol

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Experimental program
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Effect test

Embodiment 1

[0040] The configuration has figure 1 Trickle bed reactor with gas-liquid distributor shown. Wherein, the diameter of the top of the bubble cap of the gas-liquid distributor is equal to the diameter of the bottom thereof, and four rectangular slits are uniformly arranged on the lower part of the bubble cap. The catalyst in the trickle bed reactor is supported by activated carbon, and the catalyst is composed of: 15% nickel metal, 2% iron as a metal additive, 3% titanium as a metal additive, and the balance as a carrier. The mixed liquid (nitric acid: 1%wt, methanol: 99%wt) and the mixed gas (CO: 25%v / v, NO: 10%v / v, CO 2 : 15% v / v, MN: 5% v / v, N 2 : 45% v / v) into the trickle bed reactor respectively, the reaction temperature is 70°C, the reaction pressure is normal pressure, and the liquid hourly space velocity is 0.5h -1 , NO and nitric acid molar ratio of 8 reacted to generate methyl nitrite, the conversion rate of nitric acid was 95.1%.

Embodiment 2

[0042] The configuration has figure 1 Trickle bed reactor with gas-liquid distributor shown. Wherein, the top diameter of the bubble cap of the gas-liquid distributor is smaller than the bottom diameter, and the lower part of the bubble cap is uniformly provided with four slits in the shape of isosceles triangles. The catalyst in the trickle bed reactor uses silicon oxide as a carrier, and the catalyst composition is: 5% metallic nickel, 10% titanium as a metal additive, and the rest as carrier. The mixed liquid (nitric acid: 15%wt, water: 30%wt, methanol: 55%wt) and the mixed gas containing NO (CO: 30%v / v, NO: 15%v / v, CO 2 : 15% v / v, MN: 5% v / v, N 2 : 35% v / v) into the trickle bed reactor respectively, the reaction temperature is 75°C, the reaction pressure is 0.35MPa, and the liquid hourly space velocity is 6h -1 , NO and nitric acid molar ratio of 3 reacted to generate methyl nitrite, the conversion rate of nitric acid was 95.6%.

Embodiment 3

[0044] The configuration has figure 1 Trickle bed reactor with gas-liquid distributor shown. Wherein, the diameter of the top of the bubble cap of the gas-liquid distributor is equal to the diameter of the bottom, and the lower part of the bubble cap is evenly provided with 8 rectangular slits. The catalyst in the trickle bed reactor is supported by activated carbon, and the catalyst is composed of: 25% nickel metal, 1% iron as a metal additive, titanium as a metal additive, and the rest as a carrier. The mixed liquid (nitric acid: 5%wt, water: 8%wt, methanol: 87%wt) and the mixed gas containing NO (CO: 20%v / v, NO: 15%v / v, CO 2 : 10% v / v, MN: 3% v / v, N 2 : 52% v / v) into the trickle bed reactor respectively, the reaction temperature is 80 ℃, the reaction pressure is 0.6MPa, and the liquid hourly space velocity is 8h -1 , the molar ratio of NO to nitric acid was 2.5 to react to generate methyl nitrite, and the conversion rate of nitric acid was 96.5%.

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Abstract

The invention relates to a method for preparing methyl nitrite by a reaction of NO and nitric acid and methanol. By the method, the problems such as high supply cost of nitrogen oxide and severe equipment corrosion existing in present glycol preparation technology by synthesis gas are mainly solved. According to the technical scheme, a gas-phase raw material containing nitric oxide and a liquid-phase raw material containing nitric acid and methanol react in a trickle bed reactor to obtain methyl nitrite. By the technical scheme, the above problems are greatly solved. The method of the invention can be used for industrial production of methyl nitrite in the glycol preparation technology by synthesis gas.

Description

technical field [0001] The invention relates to a method for preparing methyl nitrite by reacting NO, nitric acid and methanol. Background technique [0002] Ethylene glycol (EG) is an important basic organic raw material in petrochemical industry. It is mainly used in the production of polyester, antifreeze, lubricants, plasticizers, nonionic surfactants and explosives. It has a wide range of uses. In recent years, with the increasing market demand for downstream polyester products, the world's ethylene glycol production and demand have continued to expand, and my country is the world's largest consumer of ethylene glycol, with annual consumption reaching more than 10 million tons according to statistics , import dependence of more than 70%. [0003] At present, the production routes of ethylene glycol mainly include petroleum routes and non-petroleum routes. Traditional petroleum routes consume a large amount of crude oil to produce ethylene glycol, and the economic benefi...

Claims

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Application Information

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IPC IPC(8): C07C201/04C07C203/00
CPCC07C201/04C07C203/00
Inventor 孙凤侠刘俊涛刘国强
Owner CHINA PETROLEUM & CHEM CORP
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