KR20140050229A - Equipment for freezing point analysis of carbon dioxide - Google Patents

Equipment for freezing point analysis of carbon dioxide Download PDF

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KR20140050229A
KR20140050229A KR1020120116315A KR20120116315A KR20140050229A KR 20140050229 A KR20140050229 A KR 20140050229A KR 1020120116315 A KR1020120116315 A KR 1020120116315A KR 20120116315 A KR20120116315 A KR 20120116315A KR 20140050229 A KR20140050229 A KR 20140050229A
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carbon dioxide
gas
refrigerant
pressure
methane
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KR1020120116315A
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Korean (ko)
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KR102044263B1 (en
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강동억
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대우조선해양 주식회사
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—Specially adapted to detect a particular component
    • G01N33/004—Specially adapted to detect a particular component for CO, CO2
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference

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  • Health & Medical Sciences (AREA)
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Abstract

Disclosed is a carbon dioxide condensation point analyzer. An apparatus for analyzing carbon dioxide condensation point of the present invention, the apparatus for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of the gas containing carbon dioxide, the gas supply unit for supplying a gas containing carbon dioxide; A refrigerant supply unit to which a refrigerant for condensing carbon dioxide contained in the gas is supplied; And a freezing chamber part in which a gas containing carbon dioxide is supplied to condense carbon dioxide by heat exchange with a refrigerant.

Description

Equipment For Freezing Point Analysis Of Carbon Dioxide

The present invention relates to a carbon dioxide condensation point analysis device, and more particularly, to a carbon dioxide condensation point analysis device that can analyze the condensation point of carbon dioxide according to carbon dioxide concentration or pressure while condensing gas containing carbon dioxide with liquid nitrogen. .

Lower methane gas sources, such as those produced by organic material corrosion, which are used as useful energy sources, include gases from landfills and anaerobic submergers that produce "biogas" consisting primarily of methane and carbon dioxide. Various traces of impurities, oxygen and nitrogen can also be included in the biogas, and both the methane and carbon dioxide components in the biogas are potentially valuable products if properly purified. Thus, there is a need to obtain the energy value of biogas while eliminating environmental and safety risks. Biogas from landfills and immersers have been attempted, but this methane gas source has not been used because of the problem of effectively purifying the gas, ie removing trace amounts of harmful substances, and then effectively separating carbon dioxide from the methane component. About ½ to ½ of the biogas stream resulting from anaerobic corrosion of organic matter is carbon dioxide.

Thus, the volumetric energy amount of the unrefined biogas stream is substantially less than that of pipeline natural gas. Thus, unrefined biogas cannot be introduced into gas pipelines or readily used in conventional installations without processing to remove carbon dioxide and other impurities in the gas mixture. A number of biogas source purification systems have been proposed. Separation systems based on membranes, pressure swing adsorption, temperature swing adsorption, chemical adsorption and cryogenic processes have all been reported. Each of these systems has the potential to successfully purify biogas where large volumes of biogas are available for processing or where final methane purity of up to 95% is acceptable.

The harsh, corrosive, continuous working environment at landfills limits the effectiveness of the system, requiring maintenance, maintenance, or chemical additives. Complex systems generally cost a lot of capital and maintenance. In principle, biogas can be cryogenically separated into its components using distillation techniques. Unfortunately, the distillation technique of biogas mixtures of carbon dioxide and methane is more difficult because of the many unique features of the phases present in the equilibrium mixture. Cryogenic separation can generally be subdivided into continuous and non-continuous (batch) approaches. Continuous cryogenic systems utilize areas or regions in which carbon dioxide and methane are continuously separated from each other through phase differences between components. For example, to achieve a purity of methane> 98% at a constant pressure of 700 psia or less, the solid CO 2 that is formed immediately must be separated from the mixture feed stream. Operation below the critical point of the mixture is required to maintain distinct phases to allow phase separation. The range of temperature and pressure values available for this conventional cryogenic distillation is quite limited.

Various prior art methods for cryogenic separation of carbon dioxide and methane have been taught. For example, AS Holmes, et al. (US Pat. No. 4,462,814) teaches methods and apparatus for avoiding carbon dioxide solid phase in a distillation process. In a process commonly called the Ryan-Holmes process, an alkane additive such as propane or butane is used to avoid solid CO 2 formation during liquid distillation-based separation. Butane or propane is separated from CO 2 after co-distillation from CH 4 and recycled to the distillation column. Heavy hydrocarbons (C 3+) are added to the feed stream to allow operation at reduced pressure and elevated temperatures without the formation of solid CO 2 . The addition of n-butane to the feed stream allows the distillation of the mixture to occur well in the liquid-vapor phase while eliminating solid CO 2 formation in the distillation column. In addition, the critical pressure of the mixture rises, resulting in a larger range of acceptable working pressures.

However, the Ryan-Holmes process has two significant limitations for biogas purification. First, system complexity leads to large capital costs and the inability to scale up to fewer feed streams. As mentioned above, this cost is a problem in landfill recovery systems. Second, this process requires the supply of propane or heavy alkanes that are not generally present in landfills.

More recently, Potts, Jr., et al. (US Pat. No. 5,120,338) teaches a process for separating multicomponent feed streams using distillation and controllable condensation zones. This approach differs from the Ryan-Holmes process in that solid carbon dioxide is formed in a controllable manner. This solid is melted and introduced into the liquid portion of the liquid phase. The third gas phase is rich in most of the volatile component, methane, allowing its separation. By careful control of the conditions of solid formation and gas-liquid distillation, the components can be separated into three streams. In essence, this system allows for the desired product purity to be achieved without avoiding the formation of solid carbon dioxide or the use of additives. The main limitation of this process relates to its quantity. The system complexity and cost of capital costs for biogas won two hundred a day for at least 3 ft economically used. This approach is too complex and too expensive to use with a small amount of gas.

A number of techniques are also taught that utilize some cooling with a second type of separation mechanism. For example, Sweeney, et al. (US Pat. No. 5,570,582), Soffer, et al. (US Pat. No. 5,649,996) and Ojo, et al. (US Pat. No. 5,531,808) indicate that the operation of the adsorption system is at ambient temperature. The process of increasing by working at the following temperature or cryogenic temperature is taught. Lokhandwala (US Pat. No. 5,647,227) teaches a method and apparatus in which a mixture of methane, nitrogen and at least one other component (carbon dioxide) is separated. This method uses cryogenic separation which is augmented by the membrane. This system does not depend on solid phase formation or distillation which affects the separation. This complex system also has the cost and complexity of limiting its use to landfills with biogas streams of approximately 2 million ft 3 or more per day.

In U.S. Patent No. 5,642,630, Abdelmalek, et al. Describe a method for treating and separating solid landfill gas which has been claimed to produce high liquefied natural gas streams, liquefied carbon dioxide streams and compressed natural gas streams. This patent teaches the use of four-stage compressors and three flash drums that produce pressures up to 1800 psia, the use of a plurality of recycle loops to obtain chemical additives and desired products. The complexity of the system and the associated capital costs limit its usefulness in small landfills.

U.S.A. In patent 4,681,612, O'Brien, et al. Describe a cryogenic separation system that produces a fuel-grade methane product stream and any carbon dioxide product stream. This approach relies on cryogenic distillation columns, where methane is more volatile, rich in methane in overhead products. Methane is further separated from overhead products with the use of selective membranes. The bottom product contains mainly carbon dioxide with impurities which can be further purified in separate purification columns and used as product streams as needed.

A second system using chemical additives was taught by Abdelmalek (U.S. Patent No. 5,642,630). This approach uses chemical absorption to aid separation.

As described above, various methods have been proposed for separating from a gas stream containing both carbon dioxide and methane to a high purity methane and a high purity carbon dioxide product stream.

Prior to the separation process such as cryogenic separation, it is necessary to analyze the condensation point of carbon dioxide due to the difference in concentration of carbon dioxide or the pressure change in methane gas containing carbon dioxide.

However, no suitable test device or system has been proposed to analyze this.

The present invention is to solve the problems described above, to provide a carbon dioxide condensation point analysis device that can analyze the condensation point of carbon dioxide according to the difference in the concentration of carbon dioxide or the pressure change in the methane gas containing carbon dioxide.

According to an aspect of the present invention, in the device for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of the gas containing carbon dioxide,

A gas supply unit supplying the gas containing carbon dioxide;

A refrigerant supply unit to which a refrigerant for condensing carbon dioxide contained in the gas is supplied; And

Provided is a carbon dioxide condensation point analysis apparatus including a freezing chamber unit in which the gas containing carbon dioxide is supplied and the carbon dioxide is condensed by heat exchange with the refrigerant.

The freezing chamber unit has a chamber body that is insulated from the outside, a heat exchange tube provided in the chamber body, and the gas supplied from the gas supply unit flows and exchanges heat with the refrigerant, and is connected to one end of the heat exchange tube and heat exchanged. It may include a gas discharge pipe from which the gas is discharged.

The freezing chamber unit further comprises a first temperature sensor for measuring a temperature inside the chamber body, a flexible hose for discharging solid carbon dioxide condensed by heat exchange with the refrigerant in the heat exchange tube, and a check valve provided in the flexible hose. It may include.

The gas supply part includes a gas supply pipe for supplying the gas to the freezing chamber part, a first control valve provided in the gas supply pipe to regulate a supply pressure of the gas, and the gas supplied to the heat exchange pipe. It may include a first measuring system for measuring the pressure and temperature of.

The freezing chamber unit may further include a second measurement system provided in the gas discharge pipe to measure the pressure and temperature of the gas exchanged with the refrigerant.

The refrigerant supply unit includes a refrigerant injection tube for injecting the refrigerant into the freezing chamber unit, a second control valve provided in the refrigerant injection tube to adjust the injection pressure of the refrigerant, and a temperature of the refrigerant provided in the refrigerant injection tube. It may include a temperature measuring unit to measure.

The gas is methane and the refrigerant may include liquefied nitrogen.

According to another aspect of the present invention, in the method for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of methane gas containing carbon dioxide,

1) adjusting the pressure of the methane gas containing carbon dioxide into the chamber;

2) condensing carbon dioxide contained in the methane gas by controlling the injection amount of liquefied nitrogen into the chamber;

3) evacuating the methane gas and measuring the pressure of the methane gas; And

4) There is provided a carbon dioxide condensation point analysis method comprising the step of analyzing the condensation point of carbon dioxide contained in the methane gas by measuring the temperature inside the chamber in which the difference between the introduction pressure and the discharge pressure of the methane gas occurs.

The carbon dioxide condensation point analyzing apparatus of the present invention may analyze the condensation point of carbon dioxide according to the difference in the concentration of carbon dioxide or the pressure change in the methane gas containing carbon dioxide.

1 schematically illustrates an apparatus for analyzing carbon dioxide dew point according to an embodiment of the present invention.
Figure 2 is a photograph of the carbon dioxide condensation point analysis apparatus manufactured in accordance with an embodiment of the present invention.

In order to fully understand the present invention, operational advantages of the present invention, and objects achieved by the practice of the present invention, reference should be made to the accompanying drawings and the accompanying drawings which illustrate preferred embodiments of the present invention.

Hereinafter, the present invention will be described in detail with reference to the preferred embodiments of the present invention with reference to the accompanying drawings.

1 schematically illustrates an apparatus for analyzing carbon dioxide dew point according to an embodiment of the present invention.

As shown in FIG. 1, the apparatus for analyzing carbon dioxide condensation point according to an embodiment of the present invention includes a gas containing carbon dioxide in an apparatus for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of the gas containing carbon dioxide. The gas supply unit 100 to supply, the refrigerant supply unit 200 to which the refrigerant condensing the carbon dioxide contained in the gas is supplied, and the freezing chamber unit 300 to which the carbon dioxide is supplied to condense carbon dioxide by heat exchange with the refrigerant. ).

Carbon dioxide has a sublimation point of about -78 ° C at 1 atm and a boiling point of about -57 ° C at 5.185 bar. Since methane has a boiling point of about -162 ° C at 1 atm, when you lower the temperature of a mixture of carbon dioxide and methane, the methane remains gaseous but the carbon dioxide first changes into a solid or liquid depending on the pressure conditions. do. The difference in properties between these two materials can be used to separate carbon dioxide from methane.

In this embodiment, the mixed gas of methane and carbon dioxide is supplied to the freezing chamber unit 300, the refrigerant is injected, and the mixed gas is cooled, thereby analyzing the change in condensation point according to the pressure and the concentration of carbon dioxide in the mixed gas. To provide the device.

The freezing chamber part may include a chamber body 310 which is insulated from the outside, a heat exchange tube 320 provided in the chamber body 310 and flowing gas supplied from the gas supply part 100 to exchange heat with the refrigerant; It may include a gas discharge pipe 330 connected to one end of the heat exchange pipe 320 and the heat exchanged gas is discharged.

In order to accurately analyze the change in the condensation temperature, it is necessary to block the influence of the external temperature, the outside of the chamber body 310 is insulated. The chamber body 310 may be made of a material having durability against cryogenic temperatures and pressures.

The freezing chamber unit 300 includes a first temperature sensor 340 for measuring a temperature inside the chamber body 310 and a flexible hose for discharging solid carbon dioxide condensed by heat exchange with a refrigerant in the heat exchange tube 320. , And 350, and a check valve 360 provided in the flexible hose 350.

The flexible hose 350 may be connected to an end of the heat exchange tube 320 to which the gas discharge pipe 330 is connected. The flexible hose 350 may control the discharge of carbon dioxide by providing a check valve 360 to open and close.

The gas supply unit 100 includes a gas supply pipe 110 for supplying gas to the freezing chamber part 300, a first control valve 120 provided in the gas supply pipe 110 to adjust a supply pressure of the gas, and a gas supply pipe. It may include a first measuring system 130 provided in the 110 to measure the pressure and temperature of the gas supplied to the heat exchange tube (320).

The gas supply pipe 110 is connected to the heat exchange pipe 320 of the freezing chamber 300, through which the mixed gas containing carbon dioxide is supplied to the freezing chamber 300, and the pressure of the mixed gas supplied thereto. The temperature is measured in the first measuring system 130.

The freezing chamber unit 300 may further include a second measurement system 370 provided in the gas discharge pipe 330 to measure the pressure and temperature of the gas exchanged with the refrigerant.

The coolant supply unit 200 includes a coolant injection tube 210 for injecting a coolant into the freezing chamber unit 300, a second control valve 220 provided in the coolant injection tube 210 to adjust the injection pressure of the coolant; It may include a temperature measuring unit 230 provided in the refrigerant injection pipe 210 for measuring the temperature of the refrigerant.

The gas containing carbon dioxide is methane (CH 4 ) containing carbon dioxide, and the refrigerant may be liquefied nitrogen.

Nitrogen shows a boiling point of -196 ° C under l atm, a critical temperature of -147.21 ° C, and a critical pressure of 33.5 atm. Liquid nitrogen is a liquid liquefied of such nitrogen, sufficient to phase change the carbon dioxide contained in the mixed gas of this embodiment. Can act as a refrigerant.

According to another aspect of the present invention, in the method for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of methane gas containing carbon dioxide,

1) adjusting the pressure of the methane gas containing carbon dioxide into the chamber;

2) condensing the carbon dioxide contained in the methane gas by controlling the injection amount of the liquid nitrogen to the chamber;

3) exhausting methane gas and measuring the pressure of the methane gas; And

4) A carbon dioxide dew point analysis method is provided that includes analyzing a dew point of carbon dioxide contained in methane gas by measuring a temperature in a chamber in which a difference between an introduction pressure and a discharge pressure of methane gas occurs.

As described above, through the carbon dioxide condensation point analysis apparatus according to the present embodiment it is possible to analyze the condensation point of carbon dioxide according to the difference in the concentration of carbon dioxide or the pressure change in the methane gas containing carbon dioxide.

Provides basic data of carbon dioxide condensation point according to the concentration and pressure of carbon dioxide contained in methane gas, and based on this, it is possible to produce high purity methane gas and liquefied or solidified high purity carbon dioxide by separating carbon dioxide and methane contained in mixed gas. do.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention. Accordingly, such modifications or variations are intended to fall within the scope of the appended claims.

100: gas supply part
110: gas supply pipe
120: first regulating valve
130: first measuring system
200: refrigerant supply unit
210: refrigerant injection pipe
220: second regulating valve
230: temperature measuring unit
300: freezing chamber
310: chamber body
320: heat exchanger tube
330: gas discharge pipe
340: a first temperature sensor
350: flexible hose
360: check valve
370: second measuring system
371: pressure gauge
372: thermometer

Claims (8)

In the device for analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of the gas containing carbon dioxide,
A gas supply unit supplying the gas containing carbon dioxide;
A refrigerant supply unit to which a refrigerant for condensing carbon dioxide contained in the gas is supplied; And
And a freezing chamber unit in which the gas containing carbon dioxide is supplied to condense the carbon dioxide through heat exchange with the refrigerant. The method of claim 1, wherein the freezing chamber portion
An outer insulated chamber body;
A heat exchange tube provided in the chamber body and configured to exchange heat with the refrigerant by flowing the gas supplied from the gas supply unit; And
And a gas discharge pipe connected to one end of the heat exchange pipe and through which the heat exchanged gas is discharged. The method of claim 2, wherein the freezing chamber portion
A first temperature sensor measuring a temperature inside the chamber body;
A flexible hose for discharging solid carbon dioxide condensed by heat exchange with the refrigerant in the heat exchange tube; And
Carbon dioxide condensation point analysis device further comprises a check valve provided in the flexible hose. 3. The fuel cell system according to claim 2, wherein the gas supply unit
A gas supply pipe supplying the gas to the freezing chamber unit;
A first control valve provided in the gas supply pipe to adjust a supply pressure of the gas; And
And a first measurement system provided in the gas supply pipe and measuring a pressure and a temperature of the gas supplied to the heat exchange pipe. The method of claim 2, wherein the freezing chamber portion
And a second measurement system provided in a gas discharge pipe and measuring a pressure and a temperature of the gas exchanged with the refrigerant. The method of claim 1, wherein the refrigerant supply unit
A refrigerant injection tube for injecting the refrigerant into the freezing chamber unit;
A second control valve provided in the refrigerant injection pipe to adjust the injection pressure of the refrigerant; And
Carbon dioxide condensation point analysis device provided in the refrigerant injection pipe and comprises a temperature measuring unit for measuring the temperature of the refrigerant. The method of claim 1,
Wherein the gas is methane (CH 4 ), and the refrigerant contains liquid nitrogen. In the method of analyzing the carbon dioxide condensation point according to the carbon dioxide concentration or pressure of methane gas containing carbon dioxide,
1) adjusting the pressure of the methane gas containing carbon dioxide into the chamber;
2) condensing carbon dioxide contained in the methane gas by controlling the injection amount of liquefied nitrogen into the chamber;
3) evacuating the methane gas and measuring the pressure of the methane gas; And
And 4) analyzing the dew point of the carbon dioxide contained in the methane gas by measuring the temperature inside the chamber where the difference between the introduction pressure and the discharge pressure of the methane gas occurs.
KR1020120116315A 2012-10-19 2012-10-19 Equipment For Freezing Point Analysis Of Carbon Dioxide KR102044263B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101656336B1 (en) * 2015-07-15 2016-09-09 한국표준과학연구원 Apparatus and Method for Measuring Quantity of Heat for Natural Gas

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010101983A (en) * 1999-02-05 2001-11-15 크라이오퓨얼 시스템즈 인코포레이티드 Purification of natural gas by cryogenic separation
JP2009504875A (en) * 2005-08-17 2009-02-05 ガストリートメント サービシーズ ビー．ブイ． Method and apparatus for purification of a methane-rich gas stream
KR101027809B1 (en) * 2010-02-12 2011-04-07 한솔이엠이(주) Manufacturing apparatus for liquified bio methane
KR101100321B1 (en) * 2011-11-04 2011-12-30 (주)대우건설 System for purifying/upgrading and compressing biogas

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010101983A (en) * 1999-02-05 2001-11-15 크라이오퓨얼 시스템즈 인코포레이티드 Purification of natural gas by cryogenic separation
JP2009504875A (en) * 2005-08-17 2009-02-05 ガストリートメント サービシーズ ビー．ブイ． Method and apparatus for purification of a methane-rich gas stream
KR101027809B1 (en) * 2010-02-12 2011-04-07 한솔이엠이(주) Manufacturing apparatus for liquified bio methane
KR101100321B1 (en) * 2011-11-04 2011-12-30 (주)대우건설 System for purifying/upgrading and compressing biogas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101656336B1 (en) * 2015-07-15 2016-09-09 한국표준과학연구원 Apparatus and Method for Measuring Quantity of Heat for Natural Gas

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