Process and device for the low-temperature fractionation of air

Refrigeration – Cryogenic treatment of gas or gas mixture – Separation of gas mixture

Reexamination Certificate

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C062S903000

Reexamination Certificate

active

06430961

ABSTRACT:

The invention relates to a process for the low-temperature fractionation of air.
The general principles of low-temperature fractionation of air and the design of rectifier systems for nitrogen/oxygen separation with two or more columns in particular are known from the monograph “Tieftemperaturtechnik” (Low-Temperature Technology) by Hausen/Linde (2nd edition, 1985) or from an article by Latimer in Chemical Engineering Process (Vol. 63, No. 2, 1967, page 35). The pressure column (also commonly termed “high pressure column” in the United States) and low-pressure column of a two-column system generally exchange heat via a condenser/evaporator system (principal condenser), in which top gas from the pressure column is liquefied against evaporating bottom liquid from the medium-pressure column.
The rectifier system of the invention may be designed as a conventional two-column system, but also as a three-column or multicolumn system. In addition to the columns for nitrogen/oxygen separation, it may have further devices for obtaining other components of air, in particular noble gases, for example to obtain argon.
A heat exchanger which is designed as a condenser/evaporator has evaporation passages and liquefaction passages. A liquid is evaporated in the evaporation passages. They are in heat-exchanging contact with the liquefaction passages, in which a gaseous fraction condenses in indirect heat exchange with the evaporating liquid. Details of evaporation procedures are given, for example, in the monograph “Verdampfung und ihre technischen Anwendungen” [Evaporation and technical applications thereof] by Billet (1981). A condenser/evaporator may be composed of one or more heat-exchanger blocks. A condenser/evaporator system has one or more condenser/evaporators.
For decades, the low-temperature fractionation of air used almost exclusively forced circulation evaporators as condenser/evaporators. In this type of evaporator, a heat-exchanger block is arranged in a bath of the liquid which is to be evaporated. The evaporation passages are open at the top and bottom. Liquid from the bath is entrained upwards by the gas formed during the evaporation (thermosiphon effect) and flows back into the liquid bath. In this way, a natural circulation of liquid is provided purely by the evaporation operation, without mechanical energy being supplied.
For some time, falling-film evaporators have also been used as condenser/evaporators in air fractionation installations, as described, for example, in EP 681153 A or EP 410832 A. In this type of evaporator, the liquid which is to be evaporated enters the evaporation passages at the top and flows downwards as a relatively thin film along the walls which separate the evaporation passages and liquefaction passages. This type of evaporator has a particularly low pressure, loss in the evaporation passages and is therefore generally more favourable in terms of energy than a forced circulation evaporator.
However, during evaporation of an oxygen-rich liquid, total evaporation, which would lead to the evaporation passages running dry, must be prevented. For this purpose, liquid emerging from the evaporation passages is generally returned to the inlet of the evaporation passages by means of a pump. Firstly, this measure is detrimental to the energy-saving action of the falling-film evaporator; secondly, levels of undesirable constituents with a low volatility in the liquid are increased.
The invention is therefore based on the object of providing a process of the type described in the introduction and a corresponding apparatus which can be operated economically and particularly favourably in terms of operating technology and in particular have a particularly low energy consumption.
This object is achieved by the features of the characterizing part of patent claim 1. Although, as in standard falling-film evaporation, the liquid which is not evaporated in the falling-film evaporator (first section of the condenser/evaporator system), i.e. the second oxygen-rich liquid, is fed to a delivery device, for example a pump, this device does not convey the liquid back to the inlet of the evaporation passages of the same falling-film evaporator, but rather to a second section of the condenser/evaporator system. Consequently, the first section only has to carry out a relatively small part, for example 30 to 50%, preferably 38 to 42%, of the total evaporation capacity of the condenser/evaporator system. The natural proportion of liquid at the outlet of the evaporation passages of the falling-film evaporator is correspondingly high. It is thus possible to dispense completely or to a large extent with an artificial circulation of liquid. The delivery device allows the liquid which has not been evaporated for the time being to flow onwards to a second section of the condenser/evaporator system. This second section is designed completely or partially as a forced circulation evaporator, where the problem of the need for an artificial circulation of liquid does not occur, or occurs to a lesser extent.
Within the context of the invention, it has emerged that with the aid of the measures according to the invention, the volume of pumped liquid can be reduced to approximately 30%. The effect of the reduced pumping capacity on the energy balance is not restricted to the driving energy saved; rather, the benefit is based to a greater extent on the reduced introduction of heat which results from the smaller delivery volume of second oxygen-rich liquid.
In the process according to the invention, the oxygen product is preferably removed from the second section of the condenser/evaporator system, either as a gas or as a liquid. In the latter case, it is possible, if appropriate, to obtain a gaseous pressurized oxygen product in addition to a liquid oxygen product by bringing oxygen-rich liquid in the liquid state to an elevated pressure and then evaporating it against air or nitrogen (so-called internal compression).
The first section of the condenser/evaporator system of the invention may be arranged inside the low-pressure column or in a separate vessel.
The process according to the invention and the corresponding apparatus can be used for any type of nitrogen/oxygen separation, in particular independently of the purity of the products in the heads and bottoms of the columns.
The vapour which is produced in the evaporation passages of the second section of the condenser/evaporator system is preferably not exclusively or primarily removed as a gaseous oxygen product, but rather at least half of this vapour is introduced into the low-pressure column, where it is used as rising vapour. If the entire oxygen product is obtained in liquid form and/or is internally compressed it is also possible for all the gas produced in the second section of the condenser/evaporator system to be returned to the low-pressure column.
A third oxygen-rich liquid remains in the second section of the condenser/evaporator system, as the unevaporated part of the second oxygen-rich liquid. It preferably collects in the liquid bath of the or one forced circulation evaporator. In the process according to the invention, it is preferable for at least some of this third oxygen-rich liquid to be returned to the low-pressure column and/or to the evaporation passages of the first section of the condenser/evaporator system. This returning may advantageously be carried out together with the abovementioned return of vapour to the low-pressure column, as a result of a suitable line being arranged at the height of the liquid level in the bath. This at the same time regulates the liquid level in the forced circulation evaporator without additional control devices being required.
If the second section is partially designed as a second falling-film evaporator, it is additionally possible for the delivery device which is in any case present between the first and second sections additionally to be used to produce a circulation of liquid at the second falling-film evaporator.
The liquefaction passages of the condenser/evaporato

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