CN102303864B - Production method of food-grade liquid carbon dioxide product - Google Patents
Production method of food-grade liquid carbon dioxide product Download PDFInfo
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- CN102303864B CN102303864B CN2011102307167A CN201110230716A CN102303864B CN 102303864 B CN102303864 B CN 102303864B CN 2011102307167 A CN2011102307167 A CN 2011102307167A CN 201110230716 A CN201110230716 A CN 201110230716A CN 102303864 B CN102303864 B CN 102303864B
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Abstract
The invention relates to a production method of a food-grade liquid carbon dioxide product, and in particular relates to a production method of a food-grade liquid carbon dioxide product. The production method comprises: (1) first compression process; (2) dehydrocarbon process; (3) purification process; (4) second compression process; (5) liquefaction process; and (6) distillation and purification process. According to the production method of the food-grade liquid carbon dioxide product, the dehydrocarbon process and the purification process are operated under the pressure of 0.8-1.2 MPa rather than 2.3-2.8 MPa, thus pressure-resisting grade which is provided to equipment, a meter, a pipeline, a catalyst, an adsorbent and the like in the dehydrocarbon process and purification process is low, cost investment is reduced, service life is prolonged and potential safety hazard is lowered.
Description
Technical field
The production method of relate generally to carbonic acid gas of the present invention is specifically related to a kind of production method of food level liquid carbon dioxide product.
Background technology
Fig. 2 illustrates a kind of schema of production method of food level liquid carbon dioxide product, comprises the steps:
(1) compression section 30
Will be from the mechanical water that contains outside the battery limit (BL), methane, ethene, the carbon dioxide content of the impurity such as benzene is about 99.2% CO 2 raw material gas body after washing, reconcile the excessive a little oxygen mix of the chemical reaction that enters with the variable valve 2 that stands orifice-plate flowmeter 1 control, enter together pre-cooler 10 precoolings, enter compression section 30 after removing mechanical water through the first water separator 20, boost to 0.1～0.35MPa through a stage compressor 31, two stage compressor 32 boosts to 0.8～1.2MPa and three-stage compressor 33 boosts to 2.3～2.8MPa, from three-stage compressor 33 out contain methane, ethene, the carbon dioxide of the impurity such as benzene and the temperature of oxygen are 110～120 ℃, then deliver to and take off hydrocarbon operation 50.
(2) take off hydrocarbon operation 50
At first enter from the carbon dioxide that contains the impurity such as methane, ethene, benzene of compression section 30 and oxygen and to take off hydrocarbon preheater 51 and be preheating to 215～225 ℃, then be heated to 480～520 ℃ through taking off hydrocarbon well heater 52, enter at last and take off hydrocarbon reactor 53.Methane, ethene and oxygen in taking off hydrocarbon reactor 53 and contain the carbon dioxide of the impurity such as methane, ethene, benzene is that platinum and palladium, carrier are that the effect of the catalyzer of aluminum oxide issues biochemical reaction in High Temperature High Pressure and active ingredient, generates carbonic acid gas and water.When taking off hydrocarbon preheater 51 for shell and tube heat exchanger, return the shell side that takes off hydrocarbon preheater 51 from taking off hydrocarbon reactor 53 high-temperature gas out, after the carbon dioxide heat exchange that contains the impurity such as methane, ethene, benzene from compression section 30 of tube side, carry out heat exchange through heat exchanger 130 and following combined gas streams first, through watercooler 60 cooling and the second water separator 70 separation machinery water, enter cleaning section 80 again.By taking off hydrocarbon operation 50, carbonic acid gas and water have been become from most methane, conversion of ethylene in the carbon dioxide that contains the impurity such as methane, ethene, benzene of compression section 30, therefore, enter and contain the trace methane that do not carry out chemical reaction and ethene and trace oxygen and newly-generated but the second water separator 70 indissociable water vapors in the carbon dioxide of cleaning section 80.Take off hydrocarbon well heater 52 and can be electric heater.Take off hydrocarbon reactor 53 and can have the structure of general catalyticreactor.
(3) cleaning section 80
Adopt temperature swing adsorption process, many cleaner switch operatings, when a certain or several cleaners 81 are in adsorbed state, another or several cleaners 82 are in reproduced state, remaining one or several 83 of cleaners are in stand-by state, normal temperature absorption impurity, high temperature desorption impurity, by being seated in aluminum oxide in the cleaner and silica gel absorber to the trace methane that contains from the second water separator 70, ethene, oxygen, minor amount of water steam in the carbon dioxide of the impurity such as benzene and water vapour (PPM level) and micro-benzene (PPB level) impurity selective adsorption are to the trace methane that contains from the second water separator 70, ethene, oxygen, the carbon dioxide of the impurity such as benzene and water vapour purifies.
1. absorption
The carbon dioxide that contains the impurity such as trace methane, ethene, oxygen, benzene and water vapour from the second water separator 70 enters adsorption tower from cleaner 81 bottoms that are commonly referred to adsorption tower, discharge from the top of adsorption tower.In adsorption tower, sorbent material carries out active adsorption to minor amount of water steam and micro-benzene etc., make the indexs such as water in the gas of adsorption tower exit end and benzene reach respective design index or required standard, then deliver to liquefaction operation 90 and distilation operation 100, after sorbent material is adsorbed to certain hour, estimates that sorbent material approaches and stop to adsorb when saturated.
2. reverse bleeding off pressure
After adsorption step finishes, the carbon dioxide that contains the impurity such as trace methane, ethene, oxygen in the adsorption tower is discharged outside the cleaner 81 against the release of absorption direction current limliting, the pressure after finishing in the adsorption tower is near normal pressure.
3. add thermal desorption impurity
That discharges from distilation tower 101 tops of distilation operation 100 contains a small amount of uncooled carbon dioxide and a large amount of methane, ethene, the gaseous mixture of oxygen, temperature reduces after variable valve 1013 throttling expansions, enter interchanger 1012 shell sides on distilation tower 101 tops, with the flashed vapour heat exchange of in interchanger 1012 tube sides, rising, the uncooled carbon dioxide of part in the flashed vapour is condensed and falls in distilation tower 101 tower reactors, remaining then becomes above-mentioned gaseous mixture and discharges from distilation tower 101 tops, this gaseous mixture temperature after variable valve 1013 throttling expansions reduces, enter interchanger 1012 shell sides on distilation tower 101 tops, after variable valve 1014 throttling expansions, again be depressurized to 0.05MPa from interchanger 1012 shell sides gaseous mixture out, a part that merges together the combined gas streams of rear formation with the flashed vapour of discharging from spherical tank 112 enters heat exchanger 130, with the trace methane that contains that takes off hydrocarbon preheater 51 that comes autospasy hydrocarbon operation 50, ethene, oxygen, entering electric heater 140 after the carbon dioxide heat exchange of the impurity such as benzene and water vapour is heated and is warming up to 180～235 ℃, entering and being in the cleaner 81 that adds thermal desorption impurity step is in the adsorption tower, direction flushing sorbent material against absorption, make adsorbent impurity be heated desorb, sorbent material is fully regenerated, then as exhaust gas emission.
4. cool off sorbent material
After adding the end of thermal desorption impurity step, the impurity such as the adsorbent water in the cleaner 81 and benzene almost obtain complete desorb, and directly deliver to cleaner 81 with another part of combined gas streams this moment, and the sorbent materials in the cleaner 81 are cooled to≤25 ℃.
5. cleaner pressurising
The part that switches to the cleaner that is commonly referred to adsorption tower 82 of adsorbed state from reproduced state that is used to control oneself is pressurized to adsorptive pressure 2.3～2.8MPa through the carbon dioxide that contains the impurity such as trace methane, ethene and oxygen after the purifying treatment to cleaner 81, prepares to enter next time absorption.
(4) liquefaction operation 90
From the trace methane that contains after the process purifying treatment of cleaning section 80 and distilation operation 100, the part of the carbon dioxide of the impurity such as ethene and oxygen enters the entrance of the reboiler that is commonly referred to the tower reactor coil pipe 1011 of the distilation tower 101 of distilation operation 100 through orifice-plate flowmeter 1015, fully provide product liquid carbonic acid gas distilation required thermal source, discharge from the outlet of the reboiler 1011 that is commonly referred to the tower reactor coil pipe, with from the trace methane that contains after the process purifying treatment of cleaning section 80, another part of the carbon dioxide of the impurity such as ethene and oxygen, after this another part flows out from the variable valve 1016 that is subjected to orifice-plate flowmeter 1015 controls, these two portions merge together, and the first vaporizer-condenser 91 that enters liquefaction operation 90 liquefies.The low-temperature receiver of the first vaporizer-condenser 91 of liquefaction operation 90 is liquefied ammonia, in the first vaporizer-condenser 91, the carbon dioxide that contains the impurity such as trace methane, ethene and oxygen fully and liquefied ammonia carry out thermal exchange, liquefied ammonia liquid level in the first vaporizer-condenser 91 is accurately controlled by variable valve, most carbon dioxide is fully liquefied, become-23～-24 ℃ of Liquid carbon dioxides, then send into distilation operation 100.
(5) the distilation operation 100
Carry out distilation from the carbonic acid gas after the liquefaction that contains uncooled carbon dioxide and the impurity such as trace methane, ethene and oxygen of the first vaporizer-condenser 91 of liquefaction operation 90 by the tower reactor that shower nozzle 1021 vaporific sprays enter the distilation tower 101 of distilation operation 100, the impurity such as methane, ethene and oxygen and uncooled carbon dioxide distill from the carbonic acid gas after the liquefaction, be called flashed vapour, obtain temperature in the tower reactor bottom and be-21～-23 ℃ product liquid carbonic acid gas.Flashed vapour rises from tower reactor, contacts with the fog-like liquid carbonic acid gas that sprays from shower nozzle 1021, and the uncooled carbon dioxide of the part in the flashed vapour is condensed, and falls in the tower reactor; Flashed vapour continues to rise, enter interchanger 1012 tube sides on distillation distilation tower 101 tops, with the gaseous mixture heat exchange that enters interchanger 1012 shell sides after the reduction of variable valve 1013 throttling expansion temperature, the uncooled carbon dioxide of the part in the flashed vapour is condensed, and falls in the tower reactor.Flashed vapour leaves interchanger 1012 tube sides, becomes the gaseous mixture that contains a small amount of uncooled carbon dioxide and a large amount of methane, ethene, discharges from distilation tower 101 tops of distilation operation 100.Be 28～32 ℃ from the temperature after the process purifying treatment of cleaning section 80 and contain trace methane, the part of the carbon dioxide of the impurity such as ethene and oxygen enters the entrance of the reboiler that is commonly referred to the tower reactor coil pipe 1011 of the distilation tower 101 of distilation operation 100 through orifice-plate flowmeter 1015, fully provide product liquid carbonic acid gas distilation required thermal source, discharge from the outlet of the reboiler 1011 that is commonly referred to the tower reactor coil pipe, outflow temperature is-9～-11 ℃, with be 28～32 ℃ from the temperature after the process purifying treatment of cleaning section 80 and contain trace methane, another part of the carbon dioxide of the impurity such as ethene and oxygen, after this another part flows out from the variable valve 1016 that is subjected to orifice-plate flowmeter 1015 controls, these two portions merge together, and the first vaporizer-condenser 91 that enters liquefaction operation 90 liquefies.
(6) cross cooling working procedure 110
Delivered to the second vaporizer-condenser 111 of cooling working procedure 110 from the product liquid carbonic acid gas through distilation in distilation tower 101 tower reactors of distilation operation 100, the low-temperature receiver of crossing the second vaporizer-condenser 111 of cooling working procedure 110 is liquefied ammonia, in the second vaporizer-condenser 111, the temperature of product liquid carbonic acid gas further reduces, and the product liquid carbonic acid gas that is further reduced temperature is delivered to 112 storages of product liquid carbonic acid gas basin through sequencing valve.
The production method of food level liquid carbon dioxide product shown in Figure 2 has following shortcoming:
In the production method of food level liquid carbon dioxide product shown in Figure 2, taking off hydrocarbon operation 50 and cleaning section 80 all carries out after three grades of compressions of compression section 30, the top hole pressure of three-stage compressor 33 is up to 2.3～2.8MPa, this just so that equipment, instrument, pipeline, catalyzer and the sorbent material etc. that take off in hydrocarbon operation 50 and the cleaning section 80 all under higher pressure, work, the withstand voltage rank that these equipment, instrument, pipeline, catalyzer and sorbent material etc. are proposed is high, increased the cost input, reduce work-ing life, increased potential safety hazard.
Summary of the invention
The present invention will provide a kind of production method of improved food level liquid carbon dioxide product.
The production method of food level liquid carbon dioxide product of the present invention comprises the following steps:
(1) first compression section
To contain and enter the first compression section after the excessive a little oxygen of the CO 2 raw material gas body of impurity and chemical reaction is removed mechanical water through water separator, boost to 0.1～0.35MPa and two stage compressor boosts to 0.8～1.2MPa through a stage compressor, then deliver to and take off the hydrocarbon operation;
(2) take off the hydrocarbon operation
Enter from the carbon dioxide that contains impurity of the first compression section and the excessive a little oxygen of chemical reaction and to take off the hydrocarbon operation, remove methane and ethene in the carbon dioxide that contains impurity, then deliver to cleaning section;
(3) cleaning section
Adopt temperature swing adsorption process, many cleaner switch operatings, when a certain or several cleaners are in adsorbed state, remaining cleaner then is in reproduced state, normal temperature absorption impurity, high temperature desorption impurity, by the sorbent material in the cleaner that is seated in cleaning section the minor amount of water steam of the PPM level in the carbon dioxide that contains impurity that comes autospasy hydrocarbon operation and the micro-benzene of PPB level are carried out selective adsorption, the carbon dioxide that contains impurity that comes autospasy hydrocarbon operation is purified, then deliver to the second compression section;
(4) second compression sections
The carbon dioxide that contains impurity from cleaning section enters the second compression section, boosts to 2.3～2.8MPa through the compressor of the second compression section, then delivers to liquefaction operation and distilation operation;
(5) liquefaction operation
The vaporizer-condenser that enters the liquefaction operation from the carbon dioxide that contains impurity of the second compression section and distilation operation liquefies, the carbon dioxide that major part contains impurity is liquefied, and then delivers to the distilation operation with methane, ethene and the oxygen of uncooled carbon dioxide and trace;
(6) distilation operation
The distilation tower tower reactor that enters the distilation operation from the carbonic acid gas after the liquefaction that contains uncooled carbon dioxide and trace methane, ethene and oxygen of liquefaction operation is carried out distilation, these impurity such as methane, ethene and oxygen and uncooled carbon dioxide distill from the carbonic acid gas after the liquefaction, be called flashed vapour, obtain the product liquid carbonic acid gas in the tower reactor bottom.
The production method of food level liquid carbon dioxide product of the present invention, compression section in the production method of food level liquid carbon dioxide product shown in Figure 2 is changed into the first compression section and the second compression section, the first compression section is similar to the compression section in the production method of food level liquid carbon dioxide product shown in Figure 2, be positioned at take off hydrocarbon operation and cleaning section before, but high output pressure only reaches 0.8～1.2MPa, be starkly lower than the high output pressure 2.3～2.8MPa of the compression section in the production method of food level liquid carbon dioxide product shown in Figure 2, after the second compression section is positioned at and takes off hydrocarbon operation and cleaning section, output pressure reaches 2.3～2.8MPa, this is just so that take off the hydrocarbon operation and cleaning section operates under the pressure of 0.8～1.2MPa, do not operate under the pressure of 2.3～2.8MPa the compression section in the production method of food level liquid carbon dioxide product shown in Figure 2 and do not resemble, thereby to taking off the equipment of hydrocarbon operation and cleaning section, instrument, pipeline, the withstand voltage rank that catalyzer and sorbent material etc. propose is low, reduced the cost input, prolong work-ing life, reduced potential safety hazard.
Preferably, from the carbon dioxide that contains impurity of the first compression section and the excessive a little oxygen of chemical reaction at first enter take off the hydrocarbon operation take off the hydrocarbon preheater, then through taking off the hydrocarbon well heater, enter at last and take off hydrocarbon reactor.
Preferably, taking off the hydrocarbon preheater is shell and tube heat exchanger, the carbon dioxide that contains impurity and the excessive a little oxygen of chemical reaction from the first compression section at first enter the tube side that takes off the hydrocarbon preheater that takes off the hydrocarbon operation, return the shell side that takes off the hydrocarbon preheater from taking off hydrocarbon reactor high-temperature gas out.
Description of drawings
Fig. 1 is the schema of the production method of food level liquid carbon dioxide product of the present invention;
Fig. 2 is the schema of production method of a kind of food level liquid carbon dioxide product of background technology.
Embodiment
With reference to the accompanying drawings the embodiment of the production method of food level liquid carbon dioxide product of the present invention is described in detail, it is more obvious that the feature and advantage of the production method of food level liquid carbon dioxide product of the present invention will become.
Referring to Fig. 1, the production method of food level liquid carbon dioxide product of the present invention comprises the steps:
(1) first compression section 300
Will be from the mechanical water that contains outside the battery limit (BL), methane, ethene, the carbon dioxide content of the impurity such as benzene is about 99.2% CO 2 raw material gas body after washing, reconcile the excessive a little oxygen mix of the chemical reaction that enters with the variable valve 2 that stands orifice-plate flowmeter 1 control, enter together pre-cooler 10 precoolings, enter the first compression section 300 after removing mechanical water through the first water separator 20, boost to 0.1～0.35MPa and two stage compressor 32 boosts to 0.8～1.2MPa through a stage compressor 31, from two stage compressor 32 out contain methane, ethene, the carbon dioxide of the impurity such as benzene and the temperature of oxygen are 125～135 ℃, then deliver to and take off hydrocarbon operation 50.
(2) take off hydrocarbon operation 50
At first enter from the carbon dioxide that contains the impurity such as methane, ethene, benzene of the first compression section 300 and oxygen and to take off hydrocarbon preheater 51 and be preheating to 215～225 ℃, then be heated to 480～520 ℃ through taking off hydrocarbon well heater 52, enter at last and take off hydrocarbon reactor 53.Methane, ethene and oxygen in taking off hydrocarbon reactor 53 and contain the carbon dioxide of the impurity such as methane, ethene, benzene is that platinum and palladium, carrier are that the effect of the catalyzer of aluminum oxide issues biochemical reaction in High Temperature High Pressure and active ingredient, generates carbonic acid gas and water.When taking off hydrocarbon preheater 51 for shell and tube heat exchanger, return the shell side that takes off hydrocarbon preheater 51 from taking off hydrocarbon reactor 53 high-temperature gas out, after the carbon dioxide heat exchange that contains the impurity such as methane, ethene, benzene from the first compression section 300 of tube side, carry out heat exchange through heat exchanger 130 and following combined gas streams first, through watercooler 60 cooling and the second water separator 70 separation machinery water, enter cleaning section 80 again.By taking off hydrocarbon operation 50, carbonic acid gas and water have been become from most methane, conversion of ethylene in the carbon dioxide that contains the impurity such as methane, ethene, benzene of the first compression section 300, therefore, enter in the carbon dioxide of cleaning section 80 and contain trace methane and the ethene that does not carry out chemical reaction, and trace oxygen and newly-generated but the second water separator 70 indissociable water vapors.Take off hydrocarbon well heater 52 and can be electric heater.Take off hydrocarbon reactor 53 and can have the structure of general catalyticreactor.
(3) cleaning section 80
Adopt temperature swing adsorption process, many cleaner switch operatings, when a certain or several cleaners 81 are in adsorbed state, another or several cleaners 82 are in reproduced state, remaining one or several 83 of cleaners are in stand-by state, normal temperature absorption impurity, high temperature desorption impurity, by being seated in aluminum oxide in the cleaner and silica gel absorber to the trace methane that contains from the second water separator 70, ethene, oxygen, minor amount of water steam in the carbon dioxide of the impurity such as benzene and water vapour (PPM level) and micro-benzene (PPB level) impurity selective adsorption are to the trace methane that contains from the second water separator 70, ethene, oxygen, the carbon dioxide of the impurity such as benzene and water vapour purifies.
1. absorption
The carbon dioxide that contains the impurity such as trace methane, ethene, oxygen, benzene and water vapour from the second water separator 70 enters adsorption tower from cleaner 81 bottoms that are commonly referred to adsorption tower, discharge from the top of adsorption tower, in adsorption tower, sorbent material carries out active adsorption to minor amount of water steam and micro-benzene etc., make the indexs such as water in the gas of adsorption tower exit end and benzene reach respective design index or required standard, then deliver to the second compression section 150, after sorbent material is adsorbed to certain hour, estimates that sorbent material approaches and stop to adsorb when saturated.
2. reverse bleeding off pressure
After adsorption step finishes, the carbon dioxide that contains the impurity such as trace methane, ethene, oxygen in the adsorption tower is discharged outside the cleaner 81 against the release of absorption direction current limliting, the pressure after finishing in the adsorption tower is near normal pressure.
3. add thermal desorption impurity
That discharges from distilation tower 101 tops of distilation operation 100 contains a small amount of uncooled carbon dioxide and a large amount of methane, ethene, the gaseous mixture of oxygen, temperature reduces after variable valve 1013 throttling expansions, enter interchanger 1012 shell sides on distilation tower 101 tops, with the flashed vapour heat exchange of in interchanger 1012 tube sides, rising, the uncooled carbon dioxide of part in the flashed vapour is condensed and falls in distilation tower 101 tower reactors, remaining then becomes above-mentioned gaseous mixture and discharges from distilation tower 101 tops, this gaseous mixture temperature after variable valve 1013 throttling expansions reduces, enter interchanger 1012 shell sides on distilation tower 101 tops, after variable valve 1014 throttling expansions, again be depressurized to 0.05MPa from interchanger 1012 shell sides gaseous mixture out, a part that merges together the combined gas streams of rear formation with the flashed vapour of discharging from spherical tank 112 enters heat exchanger 130, with the trace methane that contains that takes off hydrocarbon preheater 51 that comes autospasy hydrocarbon operation 50, ethene, oxygen, entering electric heater 140 after the carbon dioxide heat exchange of the impurity such as benzene and water vapour is heated and is warming up to 180～235 ℃, entering and being in the cleaner 81 that adds thermal desorption impurity step is in the adsorption tower, direction flushing sorbent material against absorption, make adsorbent impurity be heated desorb, sorbent material is fully regenerated, then as exhaust gas emission.
4. cool off sorbent material
After adding the end of thermal desorption impurity step, the impurity such as the adsorbent water in the cleaner 81 and benzene almost obtain complete desorb, and directly deliver to cleaner 81 with another part of combined gas streams this moment, and the sorbent materials in the cleaner 81 are cooled to≤25 ℃.
5. cleaner pressurising
The part that switches to the cleaner that is commonly referred to adsorption tower 82 of adsorbed state from reproduced state that is used to control oneself is pressurized to adsorptive pressure 0.8～1.2MPa through the carbon dioxide that contains the impurity such as trace methane, ethene and oxygen after the purifying treatment to cleaner 81, prepares to enter next time absorption.
(4) second compression sections 150
Enter the second compression section 150 from the carbon dioxide that contains the impurity such as trace methane, ethene and oxygen after the process purifying treatment of cleaning section 80, compressed machine 151 boosts to 2.3～2.8MPa, temperature is 28～32 ℃ after cooling, delivers to liquefaction operation 90 and distilation operation 100.
(5) liquefaction operation 90
Be 28～32 ℃ from the temperature of the second compression section 150 and distilation operation 100 and contain trace methane, the part of the carbon dioxide of the impurity such as ethene and oxygen enters the entrance of the reboiler that is commonly referred to the tower reactor coil pipe 1011 of the distilation tower 101 of distilation operation 100 through orifice-plate flowmeter 1015, fully provide product liquid carbonic acid gas distilation required thermal source, discharge from the outlet of the reboiler 1011 that is commonly referred to the tower reactor coil pipe, be 28～32 ℃ with temperature from the second compression section 150 and contain trace methane, another part of the carbon dioxide of the impurity such as ethene and oxygen, after this another part flows out from the variable valve 1016 that is subjected to orifice-plate flowmeter 1015 controls, these two portions merge together, and the first vaporizer-condenser 91 that enters liquefaction operation 90 liquefies.The low-temperature receiver of the first vaporizer-condenser 91 of liquefaction operation 90 is liquefied ammonia, in the first vaporizer-condenser 91, the carbon dioxide that contains the impurity such as trace methane, ethene and oxygen fully and liquefied ammonia carry out thermal exchange, liquefied ammonia liquid level in the first vaporizer-condenser 91 is accurately controlled by variable valve, most carbon dioxide is fully liquefied, become-23～-24 ℃ of Liquid carbon dioxides, then send into distilation operation 100.
(6) the distilation operation 100
Carry out distilation from the carbonic acid gas after the liquefaction that contains uncooled carbon dioxide and the impurity such as trace methane, ethene and oxygen of the first vaporizer-condenser 91 of liquefaction operation 90 by the tower reactor that shower nozzle 1021 vaporific sprays enter the distilation tower 101 of distilation operation 100, the impurity such as methane, ethene and oxygen and uncooled carbon dioxide distill from the carbonic acid gas after the liquefaction, be called flashed vapour, obtain temperature in the tower reactor bottom and be-21～-23 ℃ product liquid carbonic acid gas.Flashed vapour rises from tower reactor, contacts with the fog-like liquid carbonic acid gas that sprays from shower nozzle 1021, and the uncooled carbon dioxide of the part in the flashed vapour is condensed, and falls in the tower reactor; Flashed vapour continues to rise, enter interchanger 1012 tube sides on distillation distilation tower 101 tops, with the gaseous mixture heat exchange that enters interchanger 1012 shell sides after the reduction of variable valve 1013 throttling expansion temperature, the uncooled carbon dioxide of the part in the flashed vapour is condensed, and falls in the tower reactor.Flashed vapour leaves interchanger 1012 tube sides, becomes the gaseous mixture that contains a small amount of uncooled carbon dioxide and a large amount of methane, ethene, discharges from distilation tower 101 tops of distilation operation 100.Be 28～32 ℃ from the temperature of the second compression section 150 and contain trace methane, the part of the carbon dioxide of the impurity such as ethene and oxygen enters the entrance of the reboiler that is commonly referred to the tower reactor coil pipe 1011 of the distilation tower 101 of distilation operation 100 through orifice-plate flowmeter 1015, fully provide product liquid carbonic acid gas distilation required thermal source, discharge from the outlet of the reboiler 1011 that is commonly referred to the tower reactor coil pipe, outflow temperature is-9～-11 ℃, be 28～32 ℃ with temperature from the second compression section 150 and contain trace methane, another part of the carbon dioxide of the impurity such as ethene and oxygen, after this another part flows out from the variable valve 1016 that is subjected to orifice-plate flowmeter 1015 controls, these two portions merge together, and the first vaporizer-condenser 91 that enters liquefaction operation 90 liquefies.
(7) cross cooling working procedure 110
Delivered to the second vaporizer-condenser 111 of cooling working procedure 110 from the product liquid carbonic acid gas through distilation in distilation tower 101 tower reactors of distilation operation 100, the low-temperature receiver of crossing the second vaporizer-condenser 111 of cooling working procedure 110 is liquefied ammonia, in the second vaporizer-condenser 111, the temperature of product liquid carbonic acid gas further reduces, and the product liquid carbonic acid gas that is further reduced temperature is delivered to 112 storages of product liquid carbonic acid gas basin through sequencing valve.
According to the embodiment of the present invention describing the present invention property and nonrestrictive description, but should be understood that in the situation that do not break away from relevant protection domain defined by the claims, those skilled in the art can make change and/or revise.
Claims (3)
1. the production method of a food level liquid carbon dioxide product comprises the following steps:
(1) first compression section
To contain and enter the first compression section after the excessive a little oxygen of the CO 2 raw material gas body of impurity and chemical reaction is removed mechanical water through water separator, boost to 0.1～0.35MPa and two stage compressor boosts to 0.8～1.2MPa through a stage compressor, then deliver to and take off the hydrocarbon operation;
(2) take off the hydrocarbon operation
Enter from the carbon dioxide that contains impurity of the first compression section and the excessive a little oxygen of chemical reaction and to take off the hydrocarbon operation, remove methane and ethene in the carbon dioxide that contains impurity, then deliver to cleaning section;
(3) cleaning section
Adopt temperature swing adsorption process, many cleaner switch operatings, when a certain or several cleaners are in adsorbed state, remaining cleaner then is in reproduced state, normal temperature absorption impurity, high temperature desorption impurity, by the sorbent material in the cleaner that is seated in cleaning section the minor amount of water steam of the PPM level in the carbon dioxide that contains impurity that comes autospasy hydrocarbon operation and the micro-benzene of PPB level are carried out selective adsorption, the carbon dioxide that contains impurity that comes autospasy hydrocarbon operation is purified, then deliver to the second compression section;
(4) second compression sections
The carbon dioxide that contains impurity from cleaning section enters the second compression section, boosts to 2.3～2.8MPa through the compressor of the second compression section, then delivers to liquefaction operation and distilation operation;
(5) liquefaction operation
The vaporizer-condenser that enters the liquefaction operation from the carbon dioxide that contains impurity of the second compression section and distilation operation liquefies, the carbon dioxide that major part contains impurity is liquefied, and then delivers to the distilation operation with methane, ethene and the oxygen of uncooled carbon dioxide and trace;
(6) distilation operation
The distilation tower tower reactor that enters the distilation operation from the carbonic acid gas after the liquefaction that contains uncooled carbon dioxide and trace methane, ethene and oxygen of liquefaction operation is carried out distilation, these impurity such as methane, ethene and oxygen and uncooled carbon dioxide distill from the carbonic acid gas after the liquefaction, be called flashed vapour, obtain the product liquid carbonic acid gas in the tower reactor bottom.
2. according to the production method of food level liquid carbon dioxide product claimed in claim 1, it is characterized in that: from the carbon dioxide that contains impurity of the first compression section and the excessive a little oxygen of chemical reaction at first enter take off the hydrocarbon operation take off the hydrocarbon preheater, then through taking off the hydrocarbon well heater, enter at last and take off hydrocarbon reactor.
3. according to the production method of food level liquid carbon dioxide product claimed in claim 2, it is characterized in that: taking off the hydrocarbon preheater is shell and tube heat exchanger, the carbon dioxide that contains impurity and the excessive a little oxygen of chemical reaction from the first compression section at first enter the tube side that takes off the hydrocarbon preheater that takes off the hydrocarbon operation, return the shell side that takes off the hydrocarbon preheater from taking off hydrocarbon reactor high-temperature gas out.
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| CN107174832A (en) * | 2017-06-15 | 2017-09-19 | 重庆川茂化工科技有限公司 | Gas purification high-purity distillation technology and equipment |
| CN114768422A (en) * | 2022-04-24 | 2022-07-22 | 惠州凯美特气体有限公司 | Method and equipment for removing impurities by using gaseous carbon dioxide |
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