Method for industrially preparing high-purity carbon monoxide through formic acid dehydration

A carbon monoxide and formic acid technology, applied in directions such as carbon monoxide, can solve the problems of low carbon monoxide purity, inability to continuously produce, and high production costs, and achieve the effects of safe, stable and reliable operation, saving purchase costs, and reducing purchase costs.

CN105084359AActive Publication Date: 2015-11-25BEIJING HUANYU JINGHUI CITY GAS TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2015-11-25

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Abstract

The invention relates to a method for industrially preparing high-purity carbon monoxide through formic acid dehydration. The method includes the steps that (1) formic acid is dehydrated into carbon monoxide under the concentrated sulfuric acid co-heating condition; (2) the generated carbon monoxide is purified to obtain the carbon monoxide with the purity being 99.999%; (3) dilute sulfuric acid generated by dehydration reaction is subjected to vacuum concentration, so that the dilute sulfuric acid continues participating in the reaction and being recycled, and acidic waste water generated in the reaction serves as a cooling medium and continues being recycled after being neutralized. The method achieves continuous feeding, continuous discharging, vacuum concentration of the dilute sulfuric acid and recycling of the sulfuric acid and the waste water. An advanced PLC control system is arranged, and production can be converted into industrial continuous production. Investment intensity is low, production cost is low, operation is safe, stable and reliable, and the technology saves energy and is environmentally friendly.
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Description

technical field

[0001] The invention relates to a method for preparing high-purity carbon monoxide, more specifically, the invention relates to the industrial production of high-purity carbon monoxide by using formic acid under concentrated sulfuric acid dehydration conditions. Background technique

[0002] As an important organic chemical raw material, carbon monoxide can be used in the preparation of ammonia, phosgene, alcohols, acids, anhydrides, esters, aldehydes, ether amines, alkanes and olefins, various homogeneous reaction catalysts, and the extraction of high-purity nickel. High-purity (99.99%) carbon monoxide is mainly used in the etching of chips in the semiconductor field, in the production of polycrystalline diamond films, to provide carbon sources for chemical vapor deposition processes, for pharmaceutical intermediates, standard gas preparation, carbon monoxide lasers, Environmental monitoring and scientific research and other fields.

[0003] At present, the...

Examples

Embodiment 1

[0052] (1) Dehydration reaction: 84% formic acid is divided into three paths with a speed of 256Kg / h by a metering pump and dripped into the 80% concentrated sulfuric acid in the dehydration tower tray of the dehydration reactor at the same time. After cooling, the concentrated sulfuric acid enters the dehydration tower again at 500Kg / h to dehydrate with formic acid at 75°C to generate CO and H 2 O; Concentrated sulfuric acid must supplement evaporation loss of 5%, namely: 10Kg / h.

[0053] (2) The carbon monoxide gas generated in step (1) is defoamed by the wire mesh demister made of PTFE material at the top of the dehydration tower, and defoamed by the wire mesh demister made of S30408 ​​material in the alkali washing tower, and then enters the alkali washing containing NaOH aqueous solution The tower neutralizes the saturated acidic water vapor in the carbon monoxide gas, and the neutral carbon monoxide is then passed through a chiller at a temperature of 2-3°C to remove fre...

Embodiment 2

[0058] Except for the following parameters, the method and process used are the same as in Example 1.

[0059] Concentration of formic acid: 87%

[0060] Dehydration reaction temperature: 78°C

[0061] The rate at which the concentrated sulfuric acid enters the dehydration reaction tower is: 550Kg / h

[0062] The temperature to which the concentrated sulfuric acid is cooled is: 75°C

[0063] Finally, after purification, carbon monoxide with a purity of 99.999% was obtained, and the conversion rate of formic acid was 62.8%.

Embodiment 3

[0065] Except for the following parameters, the method and process used are the same as in Example 1.

[0066] Concentration of formic acid: 90%

[0067] Dehydration reaction temperature: 80°C

[0068] The rate at which the concentrated sulfuric acid enters the dehydration reaction tower is: 600Kg / h

[0069] The temperature to which the concentrated sulfuric acid is cooled is: 80°C

[0070] Finally, after purification, carbon monoxide with a purity of 99.99% was obtained, and the conversion rate of formic acid was 61.8%.

[0071] According to the acidity degree and temperature conditions of each stage, the present invention selects materials and customizes equipment to meet the requirements of working conditions, and achieves safe and reliable production, stable and simple operation, environmental protection, energy saving, low cost, high purity of carbon monoxide obtained, and high conversion rate of formic acid . The invention can generate remarkable benefits and has goo...