CN217578331U - Production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas - Google Patents
Production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas Download PDFInfo
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- CN217578331U CN217578331U CN202121465227.5U CN202121465227U CN217578331U CN 217578331 U CN217578331 U CN 217578331U CN 202121465227 U CN202121465227 U CN 202121465227U CN 217578331 U CN217578331 U CN 217578331U
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Abstract
The utility model discloses a synthetic ammonia tail gas preparation electronic grade carbon monoxide's apparatus for producing, including desulfurizing tower, activated carbon absorber, oxygen-removing device, alkali wash ware, condenser, take off light rectifying column, take off heavy rectifying column, membrane press and gas cylinder, the desulfurizing tower communicates in activated carbon absorber, and activated carbon absorber communicates in oxygen-removing device, and oxygen-removing device communicates in alkali wash ware, and alkali wash ware passes through the condenser and communicates in taking off light rectifying column, takes off light rectifying column and communicates in taking off heavy rectifying column, and it communicates in gas cylinder to take off heavy rectifying column through the membrane press. The utility model is provided with a desulfurizing tower, an active carbon adsorber, a deoxygenator and an alkali washing device, adopts a plurality of multi-level impurity removal steps to improve the removal effect of other gases, improves the purity of carbon monoxide, reaches high-purity electronic grade 5N carbon monoxide, and realizes the high-value utilization of the synthetic ammonia tail gas; the utility model discloses do not produce the spent acid in the technology, it is not high to the requirement of equipment and container like this, also can not produce the gaseous impurity that pollutes the product simultaneously.
Description
Technical Field
The utility model belongs to the technical field of the high-purity gas preparation technique and specifically relates to a production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas.
Background
Most of the synthetic ammonia industry needs to utilize the synthesis gas generated in the coal chemical industry to obtain high-purity hydrogen through conversion and purification, and in the process of purifying hydrogen raw materials, tail gas rich in carbon monoxide can be produced, and most of the tail gas is used as fuel or directly discharged into the atmosphere, so that certain waste and pollution are caused. On the other hand, electronic grade carbon monoxide is mainly used in the fields of etching of chips in the semiconductor field, production of polycrystalline diamond films, carbon source supply for chemical vapor deposition process, medical intermediates, standard gas preparation, carbon monoxide lasers, environmental monitoring, scientific research and the like, and a large amount of electronic grade carbon monoxide gas is required in the fields.
In view of the above problems, the prior art discloses some carbon monoxide preparation technical solutions, as follows:
1. for example, the Chinese patent discloses a method and a device for preparing hydrogen and high-purity carbon monoxide by separating synthesis gas (publication number: CN 104528647A), wherein the synthesis gas is pretreated mixed gas; the method comprises the following steps: h2 and low-boiling-point impurities are separated from the top of the tower through rectification, CH4, O2 and high-boiling-point impurities are separated from the bottom of the tower through secondary rectification, N2 and high-boiling-point impurities which are not removed are separated from the top of the tower through tertiary rectification, and CO is separated from the bottom of the tower through tertiary rectification; wherein the energy transfer process accompanied by the process is realized by the absorption and release of heat of the N2 circulation loop obtained by the separation. The utility model also provides a device of above-mentioned method, mainly include dehydrogenation tower C1, deoxidation-methane tower C2 and denitrogenation tower C3's continuous rectification equipment and the relevant equipment that realizes energy transfer. The utility model overcomes the defect of traditional method, saved the equipment investment, reduced the energy consumption, improved the product added value, realized the circular economy effect.
2. For example, chinese patent discloses a system and a method for preparing high-purity carbon monoxide and hydrogen-rich CO-production liquid methane (publication number: CN 105865147B), the system mainly comprises a raw material gas purification unit, a low-temperature liquefaction separation unit, a CO product compressor and a mixed refrigerant compressor; the low temperature liquefaction separator unit include main heat exchanger, wash methane tower, dehydrogenation tower, demethanizer and denitrogenation tower, dehydrogenation tower bottom be equipped with first evaporimeter, demethanizer tower bottom be equipped with second evaporimeter, top of the tower and be equipped with first condenser, denitrogenation tower bottom be equipped with third evaporimeter, top of the tower be equipped with the second condenser, the utility model discloses a when this four tower processes obtain high-purity rich H2 and CO product, can obtain high-purity liquid methane, the device is strong to the adaptability of feed gas, has reduced the requirement of device to feed gas impurity, according to the pressure of CO product gas, takes out partly CO circulation as the cold source and the heat source of rectifying column from CO compressor's final stage or middle stage, has cancelled nitrogen compressor and expander, and equipment is less, invests for a short time.
3. Chinese patent discloses an energy-saving emission-reducing refining method of high-purity carbon monoxide (publication number: CN 101723365B), coke, carbon dioxide and oxygen are used as raw materials to prepare raw gas, the raw gas is cooled and then enters an electric tar remover, the obtained raw gas directly enters a 1-stage cylinder in a multi-stage compressor for pressurization, under the action of a hydrolysis catalyst, COS in the raw gas is decomposed into CO2 and H2S, then coarse desorption is carried out, the COS is reduced to be below 300 x 10 < -6 >, the raw gas after coarse desulfurization returns to a 2-3-stage cylinder in the multi-stage compressor, the gas after pressurization enters a pressure swing adsorption device (VPSA) to enable the H2S content to be less than 20 x 10 < -6 >, the COS content to be (20-50) x 10 < -6 >, then enters a fine desulfurization tower, fine desulfurization is carried out under the action of the catalyst, and the gas at the moment, namely, the high-purity CO gas at the outlet, the content is 97-98%. The toxic gases COS and CO2 in the whole process flow are zero-discharged, and the environment is improved.
Although the technical scheme can prepare high-purity carbon monoxide to a certain degree, the following problems exist:
1. the purity of the produced carbon monoxide is unstable, and the produced carbon monoxide cannot be used for producing electronic special gas, the quality of the electronic special gas is required to be very stable, and the removal of impurities such as sulfide in the synthesis gas is not mentioned;
2. in some preparation processes, waste acid reaction is generated, the requirement of high temperature on the material of equipment and containers is high, and concentrated sulfuric acid corrosion is easy to generate hydrogen impurities to further pollute products;
3. the purity of the prepared carbon monoxide is not high, only 97-98% of the carbon monoxide can be prepared, and the high purity requirement of electronic grade carbon monoxide cannot be met.
Therefore, a production device for preparing electronic-grade carbon monoxide from the synthesis ammonia tail gas is necessary for solving the problems.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects in the prior art, the utility model aims to provide a production device for preparing electronic-grade carbon monoxide by using synthesis ammonia tail gas, which aims to solve the problems.
The utility model provides a synthetic ammonia tail gas preparation electronic grade carbon monoxide's apparatus for producing, includes desulfurizing tower, activated carbon absorber, deoxygenator, alkali wash ware, condenser, takes off light rectifying column, takes off heavy rectifying column, membrane press and gas charging bottle, the desulfurizing tower communicate in the activated carbon absorber, the activated carbon absorber communicate in the deoxygenator, the deoxygenator communicate in the alkali wash ware, the alkali wash ware pass through the condenser communicate in take off light rectifying column, take off light rectifying column communicate in take off heavy rectifying column, take off heavy rectifying column pass through the membrane press communicate in the gas charging bottle.
Preferably, the desulfurization tower is packed with a desulfurizing agent.
Preferably, the activated carbon adsorber is filled with an activated carbon adsorbent.
Preferably, the deoxygenator is provided with a deoxygenation tower and a deoxygenation layer, the deoxygenation layer is installed in the deoxygenation tower, the deoxygenation layer is filled with a deoxidizer, one end of the deoxygenation tower is provided with an air inlet, the other end of the deoxygenation tower is provided with an air outlet, and the air inlet and the air outlet are provided with filter screens.
Preferably, the alkali scrubber comprises a multi-stage spray scrubber, the spray scrubber comprises a kettle bottom, a washing pipe, a circulating pump, a defogging layer and a spray head, the washing pipe is connected to the upper portion of the kettle bottom, the defogging layer is arranged at the inner top of the washing pipe, the spray head is arranged in the washing pipe and is arranged under the defogging layer, the spray head is communicated with the lower portion of the kettle bottom through the circulating pump, and a first liquid level meter is arranged on the side edge of the kettle bottom.
Preferably, the lower side of the washing pipe is provided with a washing inlet, the top end of the washing pipe is provided with a washing outlet, and the washing pipe is filled with a packing layer.
Preferably, an in-line condenser pipe is arranged in the condenser.
Preferably, the light component removal rectifying tower comprises a first tower tank, a circulating cooling tank, a first rectifying pipe and a circulating cooling pipe, wherein the circulating cooling tank is communicated with the first tower tank through the first rectifying pipe, the circulating cooling pipe is installed in the circulating cooling tank, the middle side edge of the first rectifying pipe is communicated with a first feeding hole, the bottom of the first tower tank is provided with a first liquid phase outlet, the top of the circulating cooling tank is provided with a first gas phase outlet, and a third packing layer is filled in the first rectifying pipe; and a second liquid level meter is arranged on the side edge of the first tower tank.
Preferably, the de-heavy rectifying tower comprises a second tower tank, a circulating heating tank, a second rectifying pipe and a circulating heating pipe, the circulating heating tank is communicated with the second tower tank through the second rectifying pipe, the circulating heating pipe is installed in the circulating heating tank, the middle side edge of the second rectifying pipe is communicated with a second feeding hole, the bottom of the second tower tank is provided with a second liquid phase outlet, the top of the circulating heating tank is provided with a second gas phase outlet, and a third packing layer is filled in the second rectifying pipe; and a third liquid level meter is arranged on the side edge of the second tower tank.
A production process of a production device for preparing electronic-grade carbon monoxide by using synthesis ammonia tail gas comprises the following process steps:
s1, feeding the synthetic ammonia tail gas into a desulfurizing tower to remove sulfides;
s2, removing sulfides, and then, putting the mixture into an activated carbon absorber to remove a first impurity substance;
s3, oxygen is removed in a deoxygenator;
s4, entering an alkaline cleaner to remove second impurities;
s5, entering a condenser to remove water;
s6, then entering a light component removal rectifying tower to remove a third impurity;
s7, feeding the mixture into a heavy matter removal rectifying tower to remove a fourth impurity substance;
and S8, finally, after the gas is qualified through inspection, filling the gas into an inflation bottle through a film pressing machine.
Compared with the prior art, the utility model discloses beneficial effect:
1. the utility model discloses be provided with desulfurizing tower, active carbon adsorber, oxygen remover, alkali scrubber, condenser, take off light rectifying column, take off heavy rectifying column, adopt multiple multi-level edulcoration step to improve and get rid of the effect to other gases, improve the purity of carbon monoxide, reach high-purity electronic grade 5N carbon monoxide, realized the high value utilization of synthetic ammonia tail gas.
2. The utility model discloses do not produce the spent acid in the technology, it is not high to the requirement of equipment and container like this, also can not produce the gaseous impurity that pollutes the product simultaneously.
3. The process of the utility model can make the synthetic ammonia tail gas into purified methane for utilization, reduce carbon emission and reduce pollution to the environment.
Drawings
FIG. 1 is a structural diagram of a production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas;
FIG. 2 is a block diagram of the present invention;
FIG. 3 is a schematic diagram of an activated carbon adsorber of the present invention;
FIG. 4 is a diagram of the deoxygenator of the present invention;
FIG. 5 is a structural diagram of the alkaline cleaner of the present invention;
FIG. 6 is a view of the structure of the light component removal rectification column of the present invention;
FIG. 7 is a structural diagram of a heavy component removal rectifying tower of the present invention;
FIG. 8 is a flow chart of the production process for preparing electronic-grade carbon monoxide from the tail gas of ammonia synthesis;
reference numbers in the figures: 1. a desulfurizing tower; 2. an activated carbon adsorber; 3. a deoxygenator; 4. an alkali washing device; 6. A condenser; 6. a light component removal rectifying tower; 7. a heavy component removal rectifying tower; 8. a film press; 9. inflating the bottle; 201. a desulfurizing agent; 301. a deoxygenation tower; 302. a deoxidized layer; 303. an air inlet; 304. an air outlet; 305. a filter screen; 401. the bottom of the kettle; 402. a wash pipe; 403. a circulation pump; 404. a defogging layer; 405. a shower head; 406. a first liquid level meter; 407. a washing inlet; 408. a washing outlet; 409. a first filler layer; 601. A first drum; 602. a circulating cooling tank; 603. a first rectification pipe; 604. a first feed port; 605. A circulating cooling pipe; 606. a first vapor phase outlet; 607. a first liquid phase outlet; 608. a second level gauge; 609. a second packing layer; 701. a second drum; 702. a circulating heating tank; 703. a second rectification pipe; 704. a second feed port; 705. circulating a heating pipe; 706. a second gas phase outlet; 707. a second liquid phase outlet; 708. a third liquid level meter; 709. a third packing layer.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
The embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways as defined and covered by the claims.
As shown in fig. 1 and fig. 2 and 8, the production apparatus for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas comprises a desulfurizing tower 1, an activated carbon adsorber 2, a deoxygenator 3, an alkaline scrubber 4, a condenser 5, a light-ends removal rectifying tower 6, a heavy-ends removal rectifying tower 7, a membrane press 8 and an inflation bottle 9, wherein the desulfurizing tower 1 is communicated with the activated carbon adsorber 2, the activated carbon adsorber 2 is communicated with the deoxygenator 3, the deoxygenator 3 is communicated with the alkaline scrubber 4, the alkaline scrubber 4 is communicated with the light-ends removal rectifying tower 6 through the condenser 5, the light-ends removal rectifying tower 6 is communicated with the heavy-ends removal rectifying tower 7, and the heavy-ends removal rectifying tower 7 is communicated with the inflation bottle 9 through the membrane press 8.
Further, the desulfurizing tower 1 is filled with a desulfurizing agent.
The beneficial effects of the further technical scheme are as follows: the desulfurizing agent includes, but is not limited to, iron oxide, zinc oxide, and the like, and is used for removing sulfide.
Further, the activated carbon adsorber 2 is filled with an activated carbon adsorbent 201.
The beneficial effects of the further technical scheme are as follows: the activated carbon adsorbent 201 is prepared from carbonaceous substances such as wood, coal, fruit shells and the like, and is used for adsorbing benzene and higher hydrocarbon impurities.
Further, the deoxygenator 3 is provided with a deoxygenation tower 301 and a deoxygenation layer 302, the deoxygenation layer 302 is installed in the deoxygenation tower 301, the deoxygenation layer 302 is filled with a deoxygenation agent, one end of the deoxygenation tower 301 is provided with an air inlet 303, the other end of the deoxygenation tower 301 is provided with an air outlet 304, and the air inlet 303 and the air outlet 304 are provided with filter screens 305.
The beneficial effects of the further technical scheme are that: the deoxidizer is CO poisoning resisting deoxidizer for removing oxygen; the filter screen is used for filtering out tiny impurity.
Further, the alkali scrubber 4 comprises a multistage spray scrubber, the spray scrubber comprises a kettle bottom 401, a washing pipe 402, a circulating pump 403, a defogging layer 404 and a spray head 405, the washing pipe 402 is connected to the upper portion of the kettle bottom 401, the defogging layer 404 is installed at the inner top portion of the washing pipe 402, the spray head 405 is installed in the washing pipe 402 and is arranged below the defogging layer 404, the spray head 405 is communicated with the lower portion of the kettle bottom 401 through the circulating pump 403, and a first liquid level meter 406 is arranged on the side edge of the kettle bottom 401.
The beneficial effects of the further technical scheme are that: the kettle bottom 401 is provided with an alkaline solution (sodium hydroxide or potassium hydroxide solution), and the alkaline solution is sprayed from a spray head 404 through a circulating pump 403 to react with acidic impurities such as nitrides, sulfides and carbon dioxide in the carbon monoxide gas and then be removed.
Further, a washing inlet 407 is formed in the side edge of the lower portion of the washing pipe 402, a washing outlet 408 is formed in the top end of the washing pipe 402, and a first filler layer 409 is filled in the washing pipe 402.
Further, a row-type condensing pipe is arranged in the condenser 5.
The beneficial effects of the further technical scheme are as follows: the row-type condensing pipe cools the carbon monoxide gas, so that moisture in the carbon monoxide gas is condensed and frozen, and most of moisture is removed.
Further, the light component removal rectifying tower 6 comprises a first tower tank 601, a circulating cooling tank 602, a first rectifying pipe 603 and a circulating cooling pipe 605, wherein the circulating cooling tank 602 is communicated with the first tower tank 601 through a first rectifying pipe 603, the circulating cooling pipe 605 is installed in the circulating cooling tank 602, a first feed inlet 604 is communicated with the side edge of the middle part of the first rectifying pipe 603, a first liquid phase outlet 607 is arranged at the bottom of the first tower tank 601, a first gas phase outlet 606 is arranged at the top of the circulating cooling tank 602, and a second packing layer 609 is filled in the first rectifying pipe 603; a second liquid level meter 608 is arranged on the side of the first tower tank 601.
The beneficial effects of the further technical scheme are that: the carbon monoxide enters the light component removal rectifying tower 6, so that the carbon monoxide with high boiling point is condensed and liquefied under the cooling effect of the circulating cooling pipe, and the impurity gas with low boiling point is not liquefied, thereby playing a role in gas separation.
Further, the heavy component removal rectification tower 7 comprises a second tower tank 701, a circulation heating tank 702, a second rectification pipe 703 and a circulation heating pipe 705, wherein the circulation heating tank 702 is communicated with the second tower tank 701 through the second rectification pipe 703, the circulation heating pipe 705 is installed in the circulation heating tank 702, the middle side of the second rectification pipe 703 is communicated with a second feed inlet 704, the bottom of the second tower tank 701 is provided with a second liquid phase outlet 707, the top of the circulation heating tank 702 is provided with a second gas phase outlet 706, and the second rectification pipe 703 is filled with a third packing layer 709; a third liquid level meter 708 is arranged on the side of the second tower tank 701.
The beneficial effects of the further technical scheme are that: the carbon monoxide enters the heavy-component removal rectifying tower 7, under the cooling effect of the circulating heating pipe, the carbon monoxide with low boiling point is condensed and gasified, and the impurity gas with high boiling point is not gasified, so that the gas separation effect is realized.
A production process of a production device for preparing electronic-grade carbon monoxide by using synthesis ammonia tail gas comprises the following process steps:
s1, feeding the synthetic ammonia tail gas into a desulfurizing tower 1 to remove sulfides;
s2, removing sulfides, and then entering an activated carbon adsorber 2 to remove first impurities;
s3, oxygen is removed in the deoxygenator 3;
s4, entering an alkaline cleaner 4 to remove second impurities;
s5, entering a condenser 5 to remove moisture;
s6, then entering a light component removal rectifying tower 6 to remove a third impurity;
s7, feeding the mixture into a de-heavy distillation tower 7 to remove fourth impurities;
and S8, finally, filling the qualified gas into an inflation bottle 9 through a membrane press 8.
Wherein the first impurity is benzene and higher hydrocarbon, and the second impurity is nitride (NO, NO) 2 Etc.), sulfides (SO) 2 、COS、H 2 S, etc.) and acidic impurities such as carbon dioxide; wherein the third impurity is light component impurities such as hydrogen, nitrogen and the like; the fourth impurity substance is heavy component impurities such as moisture, carbon dioxide, methane, alkane, alkene and the like.
Compared with the prior art, the utility model discloses beneficial effect:
1. the utility model discloses be provided with desulfurizing tower 1, active carbon adsorber 2, deoxygenator 3, alkali wash ware 4, condenser 5, take off light rectifying column 6, take off heavy rectifying column 7, adopt multiple multi-layer level edulcoration step to improve and get rid of the effect to other gases, improve the purity of carbon monoxide, reach high-purity electronic grade 5N carbon monoxide, realized the high-value utilization of synthetic ammonia tail gas.
2. The utility model discloses do not produce the spent acid in the technology, it is not high to the requirement of equipment and container like this, also can not produce the gaseous impurity that pollutes the product simultaneously.
3. The process of the utility model can make the synthetic ammonia tail gas into purified methane for utilization, reduce carbon emission and reduce environmental pollution.
Wherein the tail gas of the synthesis ammonia contains N 2 :1-5％，CO:90-95％，CH 4 0.1-1% of trace oxygen, carbon dioxide, hydrogen and Sulfide (SO) 2 、COS、H 2 S, etc.), nitrides (NO, NO) 2 Etc.), alkanes and alkenes, benzenes and higher hydrocarbons.
Wherein the desulfurizing layer of the desulfurizing tower 1 contains a desulfurizing agent comprising iron oxide (Fe) 2 O 3 ) And zinc oxide (ZnO), while the sulfide in the tail gas of synthetic ammonia contains sulfur dioxide (SO) 2 ) Carbonyl sulfide (COS), H 2 S (hydrogen sulfide) reacts with a desulfurizing agent to generate water and particle impurities, so that the effect of removing ammonia gas and hydrogen sulfide is achieved, and the specific reaction process is as follows:
(1)COS+H 2 O＝H 2 S+CO 2
(2)Fe 2 O 3 +3H 2 S＝S+2FeS+3H 2 O；
(3)H 2 S+ZnO＝ZnS+2H 2 O；
(4)Fe 2 O 3 +2SO 2 +H 2 O＝2FeSO 4 +H 2 SO 4 ；
water (H2O) and elemental sulphur (S), iron sulphide (2 FeS), zinc sulphide (ZnS), iron sulphate (FeSO) are produced 4 ) And precipitating and remaining in the desulfurizing tower.
The activated carbon adsorber 2 is internally provided with an activated carbon adsorbent (made of wood, coal and fruit shell) for adsorbing impurities of benzene and higher hydrocarbons.
The deoxidizer 3 is internally provided with a deoxidizer (reduced iron powder) for resisting CO poisoning and used for removing oxygen, the oxygen reacts with the deoxidizer to further achieve the effect of removing the oxygen, and the chemical equation is as follows:
4Fe+6H 2 O+3O 2 ＝4Fe(OH) 3
2Fe(OH) 3 ＝Fe 2 O 3 +3H 2 O
the alkaline cleaner 4 is internally provided with alkaline cleaning solution, wherein the alkaline cleaning solution (sodium hydroxide or potassium hydroxide) and nitride (NO, NO) 2 ) Sulfide (SO) 2 ) And carbon dioxide (CO) 2 ) The reaction takes place and then the function of removing impurities is achieved.
The chemical reaction principle is as follows:
wherein the equation for the reaction of sodium hydroxide with nitride is:
2NaOH+3NO 2 ＝2NaNO 3 +NO+H 2 o (main reaction)
2NaOH+NO 2 +NO＝2NaNO 2 +H 2 O (side reaction);
wherein potassium hydroxide is associated with Sulfide (SO) 2 ) The chemical reaction is as follows:
SO 2 +2KOH＝K 2 SO 3 +H 2 O；
wherein the chemical reaction between sodium hydroxide and sulfide (H2S) is as follows:
small amount of sodium hydroxide: naOH + H 2 S＝＝NaHS+H 2 O
Excess of sodium hydroxide: 2NaOH solution H 2 S＝＝Na 2 S+2H 2 O
Wherein the chemical reaction of the potassium hydroxide and the carbon dioxide is as follows:
2KOH+CO 2 ＝K 2 CO 3 +H 2 O；
KOH+CO 2 ＝KHCO 3 ；
the alkaline solution obtained by the chemical reaction reacts with the second impurities to obtain liquid or precipitate, and further the effects of gas separation and impurity removal are achieved.
The membrane press 6 employs a membrane compressor.
The working principle is as follows: the synthetic ammonia tail gas enters a desulfurizing tower 1 to remove sulfide; after removing the sulfide, the mixture enters an activated carbon adsorber 2 to remove a first impurity; enters a deoxygenator 3 to remove oxygen; the second impurities are removed in an alkali washing device 4; entering a condenser 5 to remove water; then enters a light component removal rectifying tower 6 to remove a third impurity substance; the fourth impurities are removed in a de-heavy distillation tower 7; finally, the gas is filled into an inflation bottle 9 through a film pressing machine 8 after being qualified.
The purity of the electronic grade gas is usually more than 5N grade, namely more than 99.999%.
1. Wherein Sulfide (SO) 2 、COS、H 2 ) Removing; the desulfurizing agent (ferric oxide and zinc oxide) is filled in the deoxidizing tower, so that the desulfurizing agent reacts with sulfide to generate precipitate and water, and the impurity of the sulfide is removed. The reaction principle is as follows:
(1)COS+H 2 O＝H 2 S+CO 2
(2)Fe 2 O 3 +3H 2 S＝S+2FeS+3H 2 O；
(3)H 2 S+ZnO＝ZnS+2H 2 O；
(4)Fe 2 O 3 +2SO 2 ＝＝FeSO 3 +FeSO 4 ；
producing water (H) 2 O) and elemental sulphur (S), iron sulphide (2 FeS), zinc sulphide (ZnS), iron sulphate (FeSO) 4 、FeSO 3 ) And precipitating and remaining in the desulfurizing tower.
2. Wherein, the first impurities (such as benzene and higher hydrocarbons) are removed, an activated carbon adsorber (made of wood, coal and fruit shells) is arranged in the activated carbon adsorber, and the activated carbon adsorber can adsorb the benzene and higher hydrocarbons to further achieve the effect and effect of removing the first impurities;
3. wherein, oxygen is removed, the deoxidizer (anti-CO poisoning deoxidizer, reduced iron powder) is filled in the deoxidizer, the deoxidizer reacts with the oxygen to generate precipitate and water, and then the deoxidizer plays a role in oxygen removal, and the principle is as follows:
4Fe+6H 2 O+3O 2 ＝4Fe(OH) 3 ；
2Fe(OH) 3 ＝Fe 2 O 3 +3H 2 O。
4. wherein the second impurity substance (nitride (NO, NO) 2 Etc.), sulfides (SO) 2 、COS、H 2 S, etc.) and acidic impurities such as carbon dioxide); alkali wash (sodium hydroxide or potassium hydroxide) and nitride (NO, NO) 2 ) Sulfide (SO) 2 ) And carbon dioxide (CO) 2 ) The reaction is carried out to remove impurities;
the chemical reaction principle is as follows:
the equation for the reaction of sodium hydroxide and nitride is:
2NaOH+3NO 2 ＝2NaNO 3 +NO+H 2 o (main reaction)
2NaOH+NO 2 +NO＝2NaNO 2 +H 2 O (side reaction);
wherein potassium hydroxide is associated with Sulfide (SO) 2 ) The chemical reaction is as follows:
SO 2 +2KOH＝K 2 SO 3 +H 2 O；
wherein sodium hydroxide is associated with sulfide (H) 2 S) the chemical reaction is as follows:
and (2) small amount of sodium hydroxide: naOH + H 2 S＝＝NaHS+H 2 O
Excess of sodium hydroxide: 2NaOH solution H 2 S＝＝Na 2 S+2H 2 O
Wherein the chemical reaction of the potassium hydroxide and the carbon dioxide is as follows:
2KOH+CO 2 ＝K 2 CO 3 +H 2 O；
KOH+CO 2 ＝KHCO 3 ；
the alkaline washing liquid obtained by the chemical reaction reacts with the second impurities to obtain liquid or precipitate, and then the effects and effects of gas separation and impurity removal are achieved.
4. Removal of third impurities (hydrogen, nitrogen): separating the third impurities from the carbon monoxide by using a light component removal rectifying tower; the principle of the rectifying tower is as follows: the property that the vapor pressure of each component is different at the same temperature enables the light component (low-boiling-point substance) in the liquid phase to be transferred into the gas phase, and the heavy component (high-boiling-point substance) in the gas phase to be transferred into the liquid phase, thereby realizing the purpose of separation.
The principle that carbon monoxide has a higher boiling point and a higher melting point than hydrogen and nitrogen is utilized, and low-boiling-point impurities such as hydrogen, nitrogen and the like are separated from the carbon monoxide by adopting a cooling mode; the methane is liquefied by adopting a cooling mode, and other impurities are not liquefied, so that the separation purpose is achieved.
Wherein the melting point of the carbon monoxide is-205 ℃ and the boiling point is-191.5 ℃; the melting point of hydrogen is-259.2 ℃, and the boiling point is-252.77 ℃; the melting point of nitrogen is-210 ℃ and the boiling point is-196 ℃; from the above, it can be seen that the boiling point and melting point of carbon monoxide are both significantly lower than those of hydrogen and nitrogen, and carbon monoxide can be separated from hydrogen and nitrogen by cooling to-191.5 ℃.
The working principle of the light component removal rectifying tower is as follows: the carbon monoxide gas enters a circulating cooling tank in the light component removal rectifying tower to cool the carbon monoxide gas to about minus 191.5 ℃, so that the carbon monoxide gas is condensed and liquefied into liquid to be stored at the bottom of the first tower tank, and the light component gases (hydrogen and nitrogen) are low in boiling point and cannot be liquefied, and are discharged through a first gas phase outlet for aftertreatment, thereby playing a role in separating the carbon monoxide gas from other light component gases.
5. And removing fourth impurities (moisture, carbon dioxide, methane, alkane and alkene), and separating carbon monoxide from heavy component impurities (moisture, carbon dioxide, methane, alkane and alkene) by using a heavy component removal rectifying tower.
The principle that carbon monoxide is lower than the boiling points and the melting points of moisture, carbon dioxide, methane, alkane and alkene is utilized, and high boiling point impurities and melting point impurities such as moisture, carbon dioxide, methane, alkane and alkene are separated from the carbon monoxide in a heating mode; the carbon monoxide is gasified by adopting a heating mode, and other impurities are gasified, so that the separation effect is achieved.
Wherein the melting point of carbon monoxide is-205 deg.C, the boiling point is-191.5 deg.C, the boiling point of water is 100 deg.C, the melting point is 0 deg.C, the boiling point of carbon dioxide is-78.5 deg.C, and the melting point is-56.6 deg.C; methane has a melting point of-182.5 ℃ and a boiling point of-161.5 ℃ and the alkane has the lowest boiling point of methane, the olefin usually has a boiling point higher than that of carbon monoxide, for example ethylene has a boiling point of-103.9 ℃; carbon monoxide can be separated from moisture, carbon dioxide, methane, alkanes and alkenes by raising the temperature to a temperature of about-191.5 ℃.
The working principle of the heavy component removal rectifying tower is as follows: the carbon monoxide liquid enters a heavy component removal rectifying tower, the carbon monoxide is heated to the temperature of about minus 191.5 ℃ by the circulating heating tank, so that the carbon monoxide gas is discharged from a gas phase outlet and is filled into an inflation bottle through a membrane press, the heavy component gas (moisture, carbon dioxide, methane, alkane and olefin) with higher boiling point can not be gasified, and the heavy component gas is stored at the bottom of a second tower tank for post-treatment, thereby playing a role in separating the carbon monoxide gas from other heavy component impurities.
In order to more clearly illustrate the technical effects brought by the production device and the process for preparing electronic grade high-purity methane from synthesis ammonia tail gas provided by the utility model, the following example group data is provided for illustration. It should be understood that the data set forth in the following examples are only for the purpose of better illustrating the technical effect of the continuous process for the production of high purity chlorine as proposed by the present invention and are not equivalent to all experimental data.
Comparative experiment 1:
choose experiment group 1 and contrast 1-3, experiment group 1 utilizes the utility model discloses a carbon monoxide after the purification of theory of operation flow, contrast 1-3 are the carbon monoxide after the embodiment purification that utilizes reference 1-3 of background art to correspond respectively, then utilize check out test set to detect gas composition separately, and concrete experimental result is as shown in following table 1:
table 1 shows the gas content of each component after carbon monoxide purification in comparative experiment 1:
contrastive analysis 1 combines experiment group 1 and contrast group 1-3 to derive, and the purity of experiment group 1 carbon monoxide is higher than contrast group 1-3, does not detect sulphide, oxygen and heavy ends gas in experiment group 1 simultaneously, can reachs from this the technical scheme of the utility model can detach sulphide, oxygen and heavy ends gas, and the prior art scheme of contrast group can not detach sulphide, oxygen and heavy ends gas.
Comparative experiment 2: choose experiment group 1 and experiment group 2, experiment group 1 utilizes the utility model discloses a carbon monoxide after the purification of theory of operation flow, experiment group 2 does not have the deoxygenator on experiment group 1's basis, then utilizes check out test set to detect gas composition separately, and concrete experimental result is as shown in table 2 below:
table 1 shows the gas component contents of the components after carbon monoxide purification in comparative experiment 2
Comparative analysis 3: the combination of the experimental group 1 and the experimental group 2 shows that the purification purity of the experimental group 1 is high, and the experimental group 2 does not have a deoxygenator, so that a large amount of oxygen is not removed, the purity of carbon monoxide is reduced, and the removal of other impurities is reduced.
The above only is the preferred embodiment of the present invention, not limiting the scope of the present invention, all the equivalent structures or equivalent flow changes made by the contents of the specification and the drawings, or directly or indirectly applied to other related technical fields, are included in the same way in the protection scope of the present invention.
Claims (9)
1. The utility model provides a production device of synthetic ammonia tail gas preparation electronic grade carbon monoxide which characterized in that: including desulfurizing tower (1), activated carbon absorber (2), oxygen remover (3), alkali scrubber (4), condenser (5), lightness-removing rectifying column (6), weight-removing rectifying column (7), membrane press (8) and gas charging bottle (9), desulfurizing tower (1) communicate in activated carbon absorber (2), activated carbon absorber (2) communicate in oxygen remover (3), oxygen remover (3) communicate in alkali scrubber (4), alkali scrubber (4) communicate through condenser (5) in lightness-removing rectifying column (6), lightness-removing rectifying column (6) communicate in weight-removing rectifying column (7), weight-removing rectifying column (7) communicate through membrane press (8) in gas charging bottle (9).
2. The production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas as claimed in claim 1, wherein: and a desulfurizer is filled in the desulfurizing tower (1).
3. The production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas as claimed in claim 1, wherein: and the activated carbon adsorber (2) is filled with an activated carbon adsorbent.
4. The apparatus for producing electronic grade carbon monoxide from ammonia synthesis tail gas as claimed in claim 1, wherein: the deoxygenator (3) is provided with a deoxygenation tower (301) and a deoxygenation layer (302), the deoxygenation layer (302) is installed in the deoxygenation tower (301), the deoxygenation layer (302) is filled with a deoxidizing agent, one end of the deoxygenation tower (301) is provided with an air inlet (303), the other end of the deoxygenation tower (301) is provided with an air outlet (304), and the air inlet (303) and the air outlet (304) are provided with filter screens (305).
5. The production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas as claimed in claim 1, wherein: the alkali washing device (4) comprises a multistage spray type washer, the spray type washer comprises a kettle bottom (401), a washing pipe (402), a circulating pump (403), a demisting layer (404) and a spray head (405), the washing pipe (402) is connected to the upper portion of the kettle bottom (401), the demisting layer (404) is installed at the inner top of the washing pipe (402), the spray head (405) is installed in the washing pipe (402) and placed under the demisting layer (404), the spray head (405) is communicated with the lower portion of the kettle bottom (401) through the circulating pump (403), and a first liquid level meter (406) is arranged on the side edge of the kettle bottom (401).
6. The production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas as claimed in claim 5, wherein: the washing machine is characterized in that a washing inlet (407) is formed in the side edge of the lower portion of the washing pipe (402), a washing outlet (408) is formed in the top end of the washing pipe (402), and a first packing layer (409) is filled in the washing pipe (402).
7. The production device for preparing electronic-grade carbon monoxide from synthesis ammonia tail gas as claimed in claim 1, wherein: a row-type condensing pipe is arranged in the condenser (5).
8. The apparatus for producing electronic grade carbon monoxide from ammonia synthesis tail gas as claimed in claim 1, wherein: the light component removal rectifying tower (6) comprises a first tower tank (601), a circulating cooling tank (602), a first rectifying pipe (603) and a circulating cooling pipe (605), wherein the circulating cooling tank (602) is communicated with the first tower tank (601) through the first rectifying pipe (603), the circulating cooling pipe (605) is installed in the circulating cooling tank (602), the side edge of the middle of the first rectifying pipe (603) is communicated with a first feeding hole (604), a first liquid phase outlet (607) is formed in the bottom of the first tower tank (601), a first gas phase outlet (606) is formed in the top of the circulating cooling tank (602), and a second packing layer (609) is filled in the first rectifying pipe (603); a second liquid level meter (608) is arranged on the side of the first tower tank (601).
9. The apparatus for producing electronic grade carbon monoxide from ammonia synthesis tail gas as claimed in claim 1, wherein: the de-heavy rectifying tower (7) comprises a second tower tank (701), a circulating heating tank (702), a second rectifying pipe (703) and a circulating heating pipe (705), wherein the circulating heating tank (702) is communicated with the second tower tank (701) through the second rectifying pipe (703), the circulating heating pipe (705) is installed in the circulating heating tank (702), the side edge of the middle of the second rectifying pipe (703) is communicated with a second feeding hole (704), the bottom of the second tower tank (701) is provided with a second liquid phase outlet (707), the top of the circulating heating tank (702) is provided with a second gas phase outlet (706), and a third packing layer (709) is filled in the second rectifying pipe (703); and a third liquid level meter (708) is arranged on the side edge of the second tower tank (701).
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| CN113336225A (en) * | 2021-06-29 | 2021-09-03 | 湖北和远气体股份有限公司 | Production device and process for preparing electronic-grade carbon monoxide from synthetic ammonia tail gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113336225A (en) * | 2021-06-29 | 2021-09-03 | 湖北和远气体股份有限公司 | Production device and process for preparing electronic-grade carbon monoxide from synthetic ammonia tail gas |
| CN113336225B (en) * | 2021-06-29 | 2023-10-24 | 湖北和远气体股份有限公司 | Production device and process for preparing electronic grade carbon monoxide from synthetic ammonia tail gas |
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