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

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.

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...

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Problems solved by technology

[0003] At present, the preparation methods of carbon monoxide mainly include: in the iron and steel industry, coke is used to produce coke oven gas (containing carbon monoxide) on a large scale for metal reduction, but the content of carbon monoxide in the coke oven gas produced by this method is relatively low, and other impurity groups There are many points, and it is very difficult to purify to high-purity>99.99% carbon monoxide on this basis; formic acid can also produce carbon monoxide under catalyst conditions, but the problem of this method is that the cost is high and the conversion rate of formic acid is low. And hydrogen will be produced in the process, which cannot be absolutely removed; in the laboratory, carbon monoxide is prepared by dropping formic acid into concentrated sulfuric acid. The carbon monoxide produced by this method has a relatively high purity, but it cannot be produced on a large scale or continuously, and The generated waste acid is not easy to handle; Japanese patent (JP2011051852A) discloses a scheme of dehydrating formic acid under the condition of concentrated sulfuric acid and industrially preparing carbon monoxide, which realizes the recycling of sulfuric acid and solves the problem of waste acid discharge. The dilute sulfuric acid is evaporated and concentrated under the condition of 210°C, which increases the production cost and the requirements for the material of the equipment, and the purity of carbon monoxide obtained by this scheme is only 96.1%.

[0004] Therefore, the current use of formic acid and concentrated sulfuric acid to prepare carbon monoxide mainly has equipment that cannot continuously feed and discharge materials, and the production cost is high, and the purity of the obtained carbon monoxide is low.

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