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Production method of alkyl nitrite

The technology of an alkyl nitrite and a production method is applied in the directions of nitrate preparation, organic chemistry, etc., and can solve the problems of low yield of alkyl nitrite, increased energy consumption, and high energy consumption of devices

Active Publication Date: 2018-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Reboiling the tower kettle can effectively recover methyl nitrite, but at the same time, gasifying a large amount of methanol also greatly increases the energy consumption of the device
[0008] In a word, the prior art has the problems of low yield of alkyl nitrite caused by the dissolution of alkyl nitrite in the discharged alkyl alcohol solution, and high energy consumption of the device due to reactive distillation

Method used

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  • Production method of alkyl nitrite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The methyl nitrite production process of the present embodiment is used for the scale of producing 1000 tons of dimethyl oxalate per year.

[0047] Containing NO circulating gas flow rate 500Nm 3 / h, the volume composition is: NO15%, CO8%, methyl nitrite 5%, methanol 6%, N 2 was 66%. The recycle gas entering the lower section of the reactor accounts for 8% of the total.

[0048] Oxygen flow rate 13.0Nm 3 / h, the purity is 99.8v%, the rest is N 2 .

[0049] The esterification reactor is a packed tower, using Raschig ring packing with a diameter of 0.4m. The packing height of the upper section 1a is 2m. 10.6m high.

[0050] The pressure at the top of the reactor is controlled at 0.25MPag, the purity of fresh methanol is 99.9%, and 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, the temperature at the lower part of the middle section of the esterification reactor is controlled a...

Embodiment 2

[0054] The methyl nitrite production process of the present embodiment is used for the scale of producing 10,000 tons of dimethyl oxalate per year.

[0055] 4960Nm circulating air flow containing NO 3 / h, molar composition NO=15%, CO=8%, methyl nitrite=5%, methyl alcohol=6%, N 2 = 66%. The recycle gas entering the lower section of the reactor accounts for 1% of the total amount.

[0056] Oxygen flow rate 126Nm 3 / h, the purity is 99.8%, the rest is N 2 .

[0057] The esterification reactor is a packed tower, using Raschig ring packing with a diameter of 1.5m. The packing height of the upper section 1a is 2m. The packing of the middle section 1b is packed in two layers. 13.2m high.

[0058] The pressure at the top of the reactor is controlled at 0.25MPag, the purity of fresh methanol is 99.9%, and 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, the temperature of the lower part of th...

Embodiment 3

[0063] The methyl nitrite production process of the present embodiment is used for the scale of producing 100,000 tons of dimethyl oxalate per year.

[0064] 49550Nm circulating air flow containing NO 3 / h, molar composition NO=15%, CO=8%, methyl nitrite=5%, methyl alcohol=6%, N 2 = 66%. The recycle gas entering the lower section of the reactor accounts for 20% of the total.

[0065] Oxygen flow rate 1246Nm 3 / h, the purity is 99.8%, the rest is N 2 .

[0066] The diameter of the esterification reactor is 3.8m, the upper section 1a adopts valve trays, the number of trays is 10, and the plate spacing is 0.5m; the middle section 1b uses Raschig ring packing, which is packed in three layers, and the height of each layer of packing is 4m. The lower section 1c uses The height of the Raschig ring packing is 4m, and the total height of the esterification reactor is 25.2m.

[0067] The pressure at the top of the reactor is controlled at 0.1MPag, the purity of fresh methanol is 9...

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Abstract

The invention relates to a production method for alkyl nitrite. The method mainly solves the technical problems of low yield of alkyl nitrite or high energy consumption of equipment in the prior art. A technical scheme of the invention adopts a reactor which is divided into three sections, i.e., an upper section, a middle section and a lower section, wherein the middle section is a reaction section, and reaction temperature is controlled through outside-cycled cooling; the upper section is an absorption section which absorbs nitric acid and water in gaseous reaction products; and the lower section is a rectification section which recovers alkyl nitrite in liquid reaction products; thus, the problem is well solved, and the production method for alkyl nitrite can be applied in industrial production of alkyl nitrite.

Description

technical field [0001] The present invention relates to a kind of production method of 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 is costly. [0003] The traditional synthesis process of oxalate is obtained by heating oxalic acid and alcohols in toluene solvent for a long time to esterify. 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 synthes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/02C07C203/00
Inventor 杨卫胜贺来宾施德
Owner CHINA PETROLEUM & CHEM CORP
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