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Method for synthesizing alkyl nitrite

A technology of alkyl nitrite and alkyl alcohol, which is applied in the preparation of nitrite, organic chemistry, etc., can solve the problems of high investment cost, high operating cost, large reactor diameter, etc.

Inactive Publication Date: 2016-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is that the prior art has the problems of large reactor diameter, high investment cost, and high operating cost, and a new method for synthesizing alkyl nitrite is provided

Method used

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  • Method for synthesizing alkyl nitrite
  • Method for synthesizing alkyl nitrite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The methyl nitrite production process of the present embodiment is used for the scale of producing 1000 tons of dimethyl oxalate per year.

[0043] Containing NO circulating gas flow rate 500Nm 3 / h, molar composition NO=15%, CO=8%, methyl nitrite=5%, methyl alcohol=6%, N 2 = 66%.

[0044] Oxygen flow rate 12.9Nm 3 / h, the purity is 99.8% by weight, the rest is N 2 .

[0045] The esterification reactor has a diameter of 0.25m and a height of 8.2m. It is in the form of a packed tower. There are four sections of packing. The packing heights are 1 / 1 / 1 / 2m respectively. The pressure at the top of the reactor is controlled at 0.25MPag.

[0046] The purity of fresh methanol is 99.9%, the flow rate is 0.13m 3 / h, temperature 20°C. Circulating methanol 3.9m 3 / h, the circulating methanol is cooled by a heat exchanger, and the temperature of the tower tank of the esterification reactor is controlled at 45°C.

[0047] The washing tower has a diameter of 0.25m and a height ...

Embodiment 2

[0051] The methyl nitrite production process of the present embodiment is used for the scale of producing 10,000 tons of dimethyl oxalate per year.

[0052] 4960Nm circulating air flow containing NO 3 / h, molar composition NO=15%, CO=8%, methyl nitrite=5%, methyl alcohol=6%, N 2 = 66%.

[0053] Oxygen flow rate 126Nm 3 / h, the purity is 99.8%, the rest is N 2 , Feeding in four sections.

[0054] The esterification reactor has a diameter of 0.9m and a height of 14.5m. It is in the form of a packed tower. There are four sections of packing. The packing heights are 2 / 2 / 2 / 3m respectively. The pressure at the top of the reactor is controlled at 0.25MPag.

[0055] The purity of fresh methanol is 99.9%, the flow rate is 1.3m 3 / h, temperature 20°C. Circulating methanol 38.7m 3 / h, the circulating methanol is cooled by a heat exchanger, and the temperature of the tower tank of the esterification reactor is controlled at 45°C.

[0056] The washing tower has a diameter of 0.9m a...

Embodiment 3

[0060] The methyl nitrite production process of the present embodiment is used for the scale of producing 100,000 tons of dimethyl oxalate per year.

[0061] 49550Nm circulating air flow containing NO 3 / h, molar composition NO=15%, CO=8%, methyl nitrite=5%, methyl alcohol=6%, N 2 = 66%.

[0062] Oxygen flow rate 1246Nm 3 / h, the purity is 99.8%, the rest is N 2 , feeding in four stages,

[0063] The esterification reactor has a diameter of 2.6m and a height of 20.5m. It is in the form of a packed tower. There are four sections of packing. The packing heights are 3 / 3 / 3 / 4m respectively. The pressure at the top of the reactor is controlled at 0.25MPag.

[0064] The purity of fresh methanol is 99.9%, and the flow rate is 12.9m 3 / h, temperature 20°C. Circulating methanol 387.1m 3 / h, the circulating methanol is cooled by a heat exchanger, and the temperature of the tower tank of the esterification reactor is controlled at 45°C.

[0065] The washing tower has a diameter of...

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Abstract

The invention relates to a method for synthesizing alkyl nitrite to mainly solve the problems of large reactor diameter, high investment cost and high operation cost existing in the prior art. The method comprises the following steps: an oxynitride-containing gas, oxygen and a first flow of alkyl alcohol enter an esterification reactor, and flow through the reactor from top to bottom, gases and liquid flow in parallel, and contact and react with each other to obtain an alkyl alcohol-containing top kettle liquid phase material flow and an alkyl nitrite-containing tower bottom gas phase material flow; the alkyl nitrite-containing tower bottom gas phase material flow is cycled through a cycle approach; and the alkyl nitrite-containing tower bottom gas phase material flow enters the bottom of a washing tower, and is in countercurrent contact with a second flow of alkyl alcohol entering from the top of the washing tower, a washing solution obtained from the bottom of the washing tower enters the top of an esterification reactor, and an alkyl nitrite product flow can be obtained from the top of the washing tower. The method adopting the above technical scheme well solves the problems, and can be used in industrial production of the alkyl nitrite.

Description

technical field [0001] The invention relates to a method for synthesizing alkyl nitrite. Background technique [0002] Oxalate is an important organic chemical raw material, which can be used to produce various dyes, solvents, extractants and various intermediates, and is widely used in fine chemicals. In addition, oxalate can be used to prepare ethylene glycol through hydrogenation reaction, which is a new large-scale industrialized ethylene glycol synthesis process route. For a long time, ethylene glycol has been mainly prepared by petroleum route, which has a high cost. [0003] The traditional synthesis process of oxalate is obtained by heating and esterifying oxalic acid and alcohols in toluene solvent. This method has high production cost, high energy consumption, large amount of waste water discharge and serious pollution. In the 1960s, D.F.Fenton of United Petroleum Corporation found that carbon monoxide, alcohol and oxygen could directly synthesize dialkyl oxalate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00
Inventor 杨卫胜贺来宾施德
Owner CHINA PETROLEUM & CHEM CORP
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