Nitrogen rejection method and apparatus

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

Reexamination Certificate

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C062S628000, C062S927000

Reexamination Certificate

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06584803

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to a method of and apparatus for rejecting nitrogen from a feed gas stream comprising methane and nitrogen so as to form a methane product.
BACKGROUND OF THE INVENTION
It is known to extract natural gas from underground reservoirs. The natural gas often contains nitrogen. The nitrogen may be in part or totally derived from nitrogen which has been injected into the reservoir as part of an enhanced oil recovery (EOR) or enhanced gas recovery (EGR) operation. A feature of such operations is that the concentration of nitrogen in the natural gas tends to increase with the passage of time from about 5% by volume to about 60% by volume.
U.S. Pat. No. 4,415,345 discloses a process for rejecting the nitrogen from the methane in a double rectification column operating at cryogenic temperatures. A double rectification column comprises a higher pressure rectification column, a lower pressure rectification column, and a condenser-reboiler placing the top of the higher pressure rectification column in indirect heat exchange relationship with a region, usually the bottom, of the lower pressure rectification column. In the process according to U.S. Pat. No. 4,415,345 a stream of a mixture of nitrogen and methane is cooled at elevated pressure to a temperature suitable for its separation by rectification. A part of the feed gas is liquefied. The resulting gas mixture is separated by rectification in a lower pressure rectification column having a condenser-reboiler operatively associated with a bottom region thereof. The reboiling passages of the condenser-reboiler are heated by pressurised nitrogen. Typically, a part of the nitrogen is separated in a higher pressure rectification column and another part flows in a heat pump circuit to and from the top of the lower pressure rectification column. At low nitrogen levels in the feed gas, the higher pressure rectification column is by-passed and all the nitrogen for the condenser-reboiler flows in the heat pump circuit, which is separate from the main heat exchanger used to cool the feed gas stream. As the nitrogen content in the feed gas gradually increases so the higher pressure column is used to provide some of the nitrogen, replacing nitrogen from the heat pump circuit. Eventually, the heat pump circuit is closed and the higher pressure column produces all the nitrogen.
The higher pressure rectification column used in the process according to U.S. Pat. No. 4,415,345 is operated with a second condenser-reboiler at its bottom. As a consequence, there is a high vapour flow therethrough and it needs to be of a relatively large diameter even though it is operated at maximum capacity only at high nitrogen concentrations.
It is an aim of the present invention to provide a method and apparatus that keeps down the vapour traffic through the higher pressure rectification column and thereby makes it possible to keep down the diameter of this column.
SUMMARY OF THE INVENTION
According to the present invention there is provided a method of rejecting nitrogen from a feed gas stream, comprising methane and nitrogen, so as to form a methane product, the mole fraction of nitrogen in the feed gas increasing over a period of time. The method comprises cooling the feed gas stream in a main heat exchanger, rectifying the cooled feed gas stream in a double rectification column comprising a higher pressure rectification column, a lower pressure rectification column, and a condenser-reboiler placing the higher pressure rectification column in heat exchange relationship with the lower pressure rectification column, expanding at least part of the feed gas stream into the higher pressure rectification column, partially liquefying the feed gas stream upstream of the double rectification column, and periodically increasing the operating pressure of the lower pressure rectification column, in response to increases in the mole fraction of nitrogen in the feed gas.
The invention also provides apparatus for rejecting nitrogen from a feed gas stream comprising methane and nitrogen so as to form a methane product. The apparatus comprises a main heat exchanger for cooling the feed gas stream, a double rectification column for rectifying the feed gas stream comprising a higher pressure rectification column, a lower pressure rectification column, and a condenser-reboiler placing the higher pressure rectification column in heat exchange relationship with the lower pressure rectification column, and an expansion device downstream of the main heat exchanger communicating with the higher pressure rectification column, the expansion device being arranged so as, in use, to introduce a part of the feed gas stream into the higher pressure rectification column in liquid state, characterised in that there is a back pressure regulating valve associated with the lower pressure rectification column which is operable to increase the pressure in the lower pressure rectification column
As the mole fraction of nitrogen in the feed gas mixture becomes greater with the passage of time, so the flow of product methane becomes less, and so less of the feed gas mixture is liquefied against the redirect flow of the product stream. In consequence, there is a tendency for an ever increasing proportion of the feed gas mixture to enter the higher pressure rectification column in vapour state with the passage of time. Thus, in its normal operating lifetime, which may well exceed ten years or more, and last until the reservoir which is the source of the feed gas mixture is effectively exhausted, the double rectification column may have to cope with a very wide range of vapour loadings, posing considerable design problems.
The obvious solution to these problems would be to arrange for all the feed gas mixture to enter the higher pressure rectification column in vapour state. Therefore, changes in the composition of the feed gas mixture would not substantially affect the vapour loading of the higher pressure rectification column. However, one disadvantage of such a procedure, is that the vapour loading of the higher pressure rectification column would always be at a maximum.
The method and apparatus according to the invention make it possible, however, to reduce the effective range of vapour loadings that both rectification columns have to face during their operating lifetime. This is primarily because increasing the operating pressure of the lower pressure rectification brings about a concomitant increase in the operating pressure of the higher pressure rectification column. Increasing the operating pressure of the higher pressure rectification column enables it to receive more vapour per unit time for operation at a given constant percentage of flood. In addition, increasing the operating pressure of the higher pressure rectification column tends to reduce the proportion of the feed gas mixture that passes out of the expansion device in liquid state. These two factors enable the method and apparatus according to the invention to be operated with a lower range of effective vapour loadings on the higher pressure rectification column than would otherwise be possible.
Preferably, particularly when the mole fraction of nitrogen in the feed gas mixture is less than 0.15, a first flow of gas is passed as a first recycle gas flow from the lower pressure rectification column to the higher pressure rectification column. The first recycle gas flow is compressed, is cooled in the main heat exchanger, is liquefied in a further condenser-reboiler, and is introduced into the higher pressure rectification column. This counteracts a tendency for the double rectification column to be short of reflux when the mole fraction of nitrogen in the feed gas mixture is relatively low, particularly when it is 0.15 or less.
A product methane stream is preferably withdrawn in liquid state from the lower pressure rectification column, is raised in pressure, and is vaporised at least in part in the main heat exchanger. A second recycle gas flow from the lower pressure rectification column is pref

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