CN1330573C - Refining method and device for ammonia - Google Patents

Refining method and device for ammonia Download PDF

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Publication number
CN1330573C
CN1330573C CNB2004100617629A CN200410061762A CN1330573C CN 1330573 C CN1330573 C CN 1330573C CN B2004100617629 A CNB2004100617629 A CN B2004100617629A CN 200410061762 A CN200410061762 A CN 200410061762A CN 1330573 C CN1330573 C CN 1330573C
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CN
China
Prior art keywords
ammonia
aforementioned
gas
liquefied
moisture
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CNB2004100617629A
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Chinese (zh)
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CN1623900A (en
Inventor
米田隆
阪口正美
池田晶义
安部敏行
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大阳东洋酸素株式会社
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Priority to JP2003404852A priority Critical patent/JP4062710B2/en
Priority to JP2003404852 priority
Application filed by 大阳东洋酸素株式会社 filed Critical 大阳东洋酸素株式会社
Publication of CN1623900A publication Critical patent/CN1623900A/en
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Publication of CN1330573C publication Critical patent/CN1330573C/en

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/024Purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26Drying gases or vapours

Abstract

The object of this invention is to provide an ammonia refining method for efficiently removing diversified kinds of non-metallic impurities included in raw material ammonia and simplifying a continuous refining process, and to provide an apparatus therefor. The gaseous ammonia refining apparatus of this invention refines the crude gaseous ammonia containing moisture and low boiling point gaseous impurities having a boiling point lower than that of the ammonia, and is equipped with: a distillation section 3 which consists of a heat exchanger into which the crude gaseous ammonia is introduced to liquefy the gaseous ammonia by using a cooling effect; an exhaust path which is disposed in the distillation section 3 and exhausts the low boiling point gaseous impurities in a gaseous state; a vaporizer which vaporizes the liquefied ammonia discharged from the distillation section 3; moisture adsorption sections 22 and 24 which adsorb the moisture; catalyst sections 23 and 25 which separate oxygen; and a gaseous ammonia introducing path which introduces the gaseous ammonia vaporized by the vaporizer into the moisture adsorption sections 22 and 24 and the catalyst sections 23 and 25.

Description

The process for purification of ammonia and refining plant

Technical field

The present invention relates to the thick ammonia gas that contains various impurity is carried out the purified process for purification, more particularly, relate to ammonia process for purification and refining plant thereof that essential high purity ammonia gas such as semi-conductor industry, chemical industry, research unit is provided.

Background technology

Ammonia generally through being usually used in semi-conductor industry etc., is being made on-the-spot the use by raw material ammonia purified ammonia.Raw material ammonia is an ammonia factory synthetic ammonia or from using the on-the-spot recovery ammonia that reclaims etc.Except metal species, also contain the nonmetallic impurity of water, hydrogen, oxygen, carbon monoxide, carbonic acid gas, methane etc. in this raw material ammonia,, must be refined into highly purified ammonia in order in semi-conductor manufacturing etc., to use.

In the past, various researchs of removing impurities in the above-mentioned raw materials ammonia have been carried out.For example, about removing moisture, patent documentation 1-spy opens flat 9-142833 communique and discloses the method that ammonia is contacted with barium oxide and remove.In addition, to carbon monoxide and carbonic acid gas, patent documentation 2-spy opens flat 6-107412 communique and discloses the method that ammonia is contacted with nickel catalyzator and remove.

Yet as mentioned above, because contain plurality of impurities in the raw material ammonia, the discrete material that must implement to propose in patent documentation 1 or the patent documentation 2 etc. is removed method.Therefore, produce the problem that refining ammonia needs many refining steps.That is,, must make with extra care continuously in order to obtain a large amount of high purity ammonia expeditiously.The discrete refining step exists continuous treating to need the problem of large-scale refining equipment for a long time.

Summary of the invention

The 1st purpose of the present invention provides ammonia process for purification and the refining plant thereof that can remove contained multiple nonmetallic impurity in the raw material ammonia without the refining step of multistep expeditiously.In addition, the 2nd purpose provides especially can remove expeditiously and anhydrates with the impurity of oxygen, helps efficiently to carry out the ammonia process for purification and the refining plant thereof of continuous treating.In addition, but the 3rd purpose provides ammonia process for purification and the refining plant of removing multiple nonmetallic impurity purifying high-purity ammonia expeditiously and can simplifying the continuous treating operation.

The present invention finishes for solving foregoing problems, the 1st scheme of the present invention is that the thick ammonia gas that contains the boiling point lower-boiling impurity gas lower than ammonia is carried out the purified method, comprise: after the distiller that heat exchanger constitutes imports the aforementioned crude ammonia gas, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, from aforementioned distiller aforementioned lower-boiling impurity gas is directly carried out the gaseous phase exhaust, from the aforementioned crude ammonia gas, remove aforementioned lower-boiling impurity gas.

The ammonia refining method that the 2nd scheme of the present invention is aforementioned the 1st scheme, wherein, at aforementioned distiller the liquefied ammonia reservoir of storing the ammonia that liquefies is set, the lower-boiling impurity that residues in the liquefied ammonia is removed in exhaust by the liquefied ammonia in this liquefied ammonia reservoir is heated.

The 3rd scheme of the present invention is the ammonia refining method of the aforementioned the 1st or 2 schemes, wherein, and by discharging liquefied ammonia from aforementioned liquefied ammonia reservoir and gasifying by the heating part.

The 4th scheme of the present invention is that the thick ammonia gas that contains moisture and oxygen is at least carried out the purified method, is included in the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen and imports the aforementioned crude ammonia gas, removes moisture and oxygen from the aforementioned crude ammonia gas.

The 5th scheme of the present invention is that the thick ammonia gas that contains moisture and oxygen is at least carried out the purified method, comprise the water adsorption portion that at least one pair of adsorption moisture is set and the catalysing area of separated oxygen, on the one hand, aforementioned water adsorption portion and aforementioned catalysing area a side import the aforementioned crude ammonia gas, from the aforementioned crude ammonia gas, remove moisture and oxygen, on the other hand, regenerate at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area feeding reducing gas.

The ammonia refining method that the 6th scheme of the present invention is aforementioned the 5th scheme, wherein, for a pair of aforementioned water adsorption portion and the each several part of aforementioned catalysing area, alternately carry out the removing and utilizing the regeneration that feeds aforementioned reducing gas of the moisture of aforementioned crude ammonia gas and oxygen repeatedly and carry out continuous treating.

The 7th scheme of the present invention, be to containing moisture, carry out the purified method with the thick ammonia gas of the boiling point lower-boiling impurity gas lower than ammonia, comprise that first removes operation, gasification process and second is removed operation, remove in the operation described first, the distiller that constitutes at heat exchanger imports the aforementioned crude ammonia gas, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, aforementioned lower-boiling impurity gas is directly carried out the exhaust of gaseous phase from aforementioned distiller, from the aforementioned crude ammonia gas, remove aforementioned lower-boiling impurity gas, in described gasification process, discharge the ammonia that liquefies at aforementioned distiller from aforementioned distiller, pass through the heating part, make it gasification, remove in the operation described second, import the ammonia that gasifies in the aforementioned gasification process in the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen, from this ammonia, remove moisture and oxygen.

The ammonia refining method that the 8th scheme of the present invention is aforementioned the 7th scheme, remove operation comprising the 3rd, remove in the operation the described the 3rd, setting is stored in the aforementioned first liquefied ammonia reservoir of removing the ammonia that operation liquefied, lower-boiling impurity residual in the liquefied ammonia is removed in exhaust by the liquefied ammonia in this liquefied ammonia reservoir is heated, remove operation by the aforementioned the 3rd liquefied ammonia is imported aforementioned gasification process, make it gasification.

The 9th scheme of the present invention is the ammonia refining method of the aforementioned the 7th or the 8th scheme, wherein, aforementioned second removes operation comprises removing and handles and manipulation of regeneration, remove in the processing described, aforementioned water adsorption portion and aforementioned catalysing area a side who establishes a pair of aforementioned water adsorption portion and aforementioned catalysing area at least import the ammonia that gasifies in the aforementioned gas operation, from this ammonia, remove moisture and oxygen, in described manipulation of regeneration, regenerate at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area feeding reducing gas.

The ammonia refining method that the 10th scheme of the present invention is aforementioned the 9th scheme, wherein, for aforementioned a pair of aforementioned water adsorption portion and each one of aforementioned catalysing area, aforementioned the removing of alternately carrying out moisture and oxygen repeatedly handled and fed the aforementioned manipulation of regeneration of aforementioned reducing gas and carry out continuous treating.

The ammonia refining method that the 11st scheme of the present invention is aforementioned the 1st~10 any scheme, wherein, the aforementioned crude ammonia gas is raw material ammonia to be separated into liquid phase and gas phase and the gas phase composition gas that obtains.

The 12nd scheme of the present invention is that the thick ammonia gas that contains the boiling point lower-boiling impurity gas lower than ammonia is carried out the purified refining plant, the distiller that has after importing the aforementioned crude ammonia gas, utilizes cooling effect that the heat exchanger of ammonia liquefaction is constituted is established at aforementioned distiller aforementioned lower-boiling impurity gas is directly carried out gaseous phase deflated exhaust channel.

The ammonia refining device that the 13rd scheme of the present invention is aforementioned the 12nd scheme, wherein, aforementioned distiller comprises the heating unit that separates aforementioned lower-boiling impurity gas the liquefied ammonia reservoir of the thick ammonia that storage has been liquefied and the liquefied ammonia in aforementioned liquefied ammonia reservoir.

The 14th scheme of the present invention is the ammonia refining device of the aforementioned the 12nd or 13 scheme, wherein, has the gasification installation that makes the liquefied ammonia gasification that aforementioned distiller discharges.

The 15th scheme of the present invention is that the thick ammonia gas that contains moisture and oxygen is at least carried out the purified refining plant, have the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen, import the aforementioned crude ammonia gas in aforementioned water adsorption portion and aforementioned catalysing area, from the aforementioned crude ammonia gas, remove moisture and oxygen.

The 16th scheme of the present invention is that the thick ammonia gas that contains moisture and oxygen is at least carried out the purified refining plant, have the water adsorption portion of at least one pair of adsorption moisture and the catalysing area of separated oxygen, be provided with to each the aforementioned water adsorption portion and the thick ammonia gas of aforementioned catalysing area importing aforementioned crude ammonia gas and import path and import path to each the aforementioned water adsorption portion and the reducing gas of aforementioned catalysing area importing reducing gas, aforementioned water adsorption portion and aforementioned catalysing area a side import path importing aforementioned crude ammonia gas by the aforementioned crude ammonia gas, from the aforementioned crude ammonia gas, remove moisture and oxygen, on the other hand, regenerate by aforementioned reducing gas importing path feeding reducing gas at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area.

The ammonia refining device that the 17th scheme of the present invention is aforementioned the 16th scheme, have the continuous treating control part of the switch of control aforementioned crude ammonia gas importing path and reducing gas importing path, make and alternately carry out the regeneration of removing and feeding aforementioned reducing gas of the moisture and the oxygen of aforementioned crude ammonia gas repeatedly for each one of a pair of aforementioned water adsorption portion and aforementioned catalysing area.

The 18th scheme of the present invention is that the thick ammonia gas that contains moisture and the boiling point lower-boiling impurity gas lower than ammonia is carried out the purified refining plant, has to import the distiller that utilizes after the aforementioned crude ammonia gas heat exchanger that ammonia is liquefied in cooling effect to constitute, what be located at aforementioned distiller directly carries out gaseous phase deflated exhaust channel with aforementioned lower-boiling impurity gas, the gasification installation that the liquefied ammonia that aforementioned distiller is discharged gasifies, the water adsorption portion of adsorption moisture, the catalysing area of separated oxygen, the ammonia that imports aforementioned water adsorption portion and aforementioned catalysing area with the ammonia that will utilize aforementioned gasification installation gasification imports path.

The ammonia refining device that the 19th scheme of the present invention is aforementioned the 18th scheme, wherein, at aforementioned distiller the liquefied ammonia reservoir of the thick ammonia of storing aforementioned distiller liquefaction is set, aforementioned liquefied ammonia reservoir comprises the heating unit of the lower-boiling impurity that is used for the liquefied ammonia of separating residual in aforementioned liquefied ammonia reservoir.

The 20th scheme of the present invention is the ammonia refining device of the aforementioned the 18th or 19 schemes, wherein, have at least one pair of aforementioned water adsorption portion and aforementioned catalysing area, aforementioned water adsorption portion and aforementioned catalysing area at each are provided with the aforementioned ammonia importing path that imports with the ammonia of aforementioned gasification installation gasification, and aforementioned water adsorption portion and aforementioned catalysing area at each are provided with the reducing gas importing path that imports reducing gas, aforementioned water adsorption portion and aforementioned catalysing area a side import the ammonia that path imports aforementioned gasification by aforementioned ammonia, from this ammonia, remove moisture and oxygen, regenerate by aforementioned reducing gas importing path feeding reducing gas at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area on the other hand.

The ammonia refining device that the 21st scheme of the present invention is aforementioned the 20th scheme, wherein, have the continuous treating control part of the switch of aforementioned ammonia importing path of control and aforementioned reducing gas importing path, make and alternately carry out the regeneration of removing and feeding aforementioned reducing gas of the moisture and the oxygen of aforementioned crude ammonia gas repeatedly for each one of a pair of aforementioned water adsorption portion and aforementioned catalysing area.

The ammonia refining device of each that the 22nd scheme of the present invention is aforementioned the 12nd~21 scheme, wherein, the aforementioned crude ammonia gas is by raw material ammonia being separated into the gas phase composition gas that liquid phase and gas phase obtain.

If adopt the ammonia refining method of the present invention's the 1st scheme, after then can importing thick ammonia gas at the distiller that heat exchanger constitutes, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, by directly carrying out the exhaust of gaseous phase, from the aforementioned crude ammonia gas, remove aforementioned lower-boiling impurity gas from the aforementioned distiller lower-boiling impurity gas that boiling point is lower than ammonia.

In addition, the thick ammonia gas among the present invention is the raw material ammonia of gaseous phase.In addition, the lower-boiling impurity gas that above-mentioned boiling point is lower than ammonia is the hydrogen (H that is contained in the thick ammonia 2), oxygen (O 2), carbon monoxide (CO), carbonic acid gas (CO 2), nitrogen (N 2), methane (CH 4) etc.

If adopt the process for purification of the present invention's the 2nd scheme, can be in aforementioned the 1st scheme, establish the liquefied ammonia reservoir of storing the ammonia liquefied at aforementioned distiller, by the liquefied ammonia in this liquefied ammonia reservoir is heated, can exhaust remove the lower-boiling impurity that residues in the liquefied ammonia, can make with extra care more highly purified ammonia.

If adopt the process for purification of the present invention's the 3rd scheme, in the aforementioned the 1st or the 2nd scheme, owing to after aforementioned liquefied ammonia reservoir discharge liquefied ammonia, make it gasification by the heating part again, so can be gaseous phase discharges high purity purified ammonia in the aforementioned the 1st or the 2nd scheme, supply with series-operation.

If adopt the process for purification of the present invention's the 4th scheme, can import thick ammonia gas in the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen, from the aforementioned crude ammonia gas, remove moisture and oxygen at least as nonmetallic impurity.In addition, catalysing area of the present invention for example if use nickel catalyzator, not only removes deoxidation, and can remove carbon monoxide (CO).The use of this nickel catalyzator is also brought into play the same effect of removing at the catalysing area of following embodiment of the present invention.In addition, as the moisture adsorbent that is used for water adsorption of the present invention portion, preferably molecular sieve, activated alumina etc.

If adopt the process for purification of the present invention's the 5th scheme, owing to establish the water adsorption portion of at least one pair of adsorption moisture and the catalysing area of separated oxygen, aforementioned water adsorption portion and aforementioned catalysing area a side import thick ammonia gas, from the aforementioned crude ammonia gas, remove moisture and oxygen at least as nonmetallic impurity, on the other hand, aforementioned water adsorption portion and aforementioned catalysing area feeding reducing gas the opposing party are regenerated, therefore can utilize the regeneration operation to carry out the processing of removing of moisture and oxygen not interruptedly, continuously, can improve the purification efficiency of high purity ammonia.Reducing gas as regeneration is used uses hydrogen and the gas mixture of nitrogen or the gas mixture of hydrogen and autofining ammonia.

If adopt the process for purification of the present invention's the 6th scheme, owing in aforementioned the 5th scheme, each one of a pair of aforementioned water adsorption portion and aforementioned catalysing area is alternately carried out removing of the moisture of aforementioned crude ammonia gas and oxygen repeatedly and continuous treating is carried out in the regeneration of aforementioned feeding reducing gas, so purifying high-purity ammonia in a large number.

If adopt the process for purification of the present invention's the 7th scheme, owing to comprise that first removes operation, gasification process and second is removed operation, remove in the operation described first, the distiller that constitutes at heat exchanger imports the thick ammonia gas that contains moisture and the boiling point lower-boiling impurity gas lower than ammonia, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, aforementioned lower-boiling impurity gas is directly carried out the exhaust of gaseous phase from aforementioned distiller, from the aforementioned crude ammonia gas, remove aforementioned lower-boiling impurity gas, in described gasification process, discharge the ammonia that liquefies at aforementioned distiller from aforementioned distiller, make it to gasify by the heating part, remove in the operation described second, import the ammonia that aforementioned gasification process gasifies in the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen, from this ammonia, remove moisture and oxygen, so can utilize aforementioned first to remove operation and remove the boiling point lower-boiling impurity gas lower than ammonia, can utilize aforementioned second to remove operation and remove moisture and oxygen through aforementioned gasification process again, can realize the continuous treatment process of impurity, refining more highly purified ammonia.

If adopt the process for purification of the present invention's the 8th scheme, since in aforementioned the 7th scheme, comprise be provided be stored in aforementioned first remove the liquefied ammonia reservoir of the ammonia that liquefies in the operation, exhaust is removed the 3rd of the lower-boiling impurity that residues in the liquefied ammonia and is removed operation by the liquefied ammonia in this liquefied ammonia reservoir is heated, by the aforementioned the 3rd remove operation with liquefied ammonia import aforementioned gasification process make it the gasification, so also can utilize the aforementioned the 3rd to remove operation and remove through aforementioned first and remove operation and residual lower-boiling impurity can also improve refining purity.

If adopt the process for purification of the present invention's the 9th scheme, in the aforementioned the 7th or 8 scheme, aforementioned second removes that operation is included in a side's who establishes a pair of aforementioned water adsorption portion and aforementioned catalysing area at least aforementioned water adsorption portion and aforementioned catalysing area imports the ammonia of aforementioned gasification process gasification and the processing of removing of removing moisture and oxygen from this ammonia, carry out the regenerated manipulation of regeneration with aforementioned water adsorption portion and aforementioned catalysing area feeding reducing gas the opposing party, so aforementioned second removes in the operation, the aforementioned water adsorption portion by carrying out at least one side and the manipulation of regeneration of aforementioned catalysing area, utilize the regeneration operation not interrupt the from the aforementioned the 1st to second and remove the series-operation of operation, but continuous treating.

If adopt the process for purification of the present invention's the 10th scheme, owing to aforementioned the removing of in aforementioned the 9th scheme each one of aforementioned a pair of aforementioned water adsorption portion and aforementioned catalysing area alternately being carried out moisture and oxygen repeatedly handled and the aforementioned manipulation of regeneration of aforementioned feeding reducing gas is carried out continuous treating, so purifying high-purity ammonia in a large number.

If adopt the process for purification of the present invention's the 11st scheme, because the aforementioned crude ammonia gas is used raw material ammonia is separated into the gas phase composition gas that liquid phase and gas phase obtain, so utilize liquid phase to contain the character of moisture and metal species impurity in a large number, with the few vapor phase ammonia of moisture and metal species impurity part content as refining starting raw material, carry out refinement treatment by the process for purification of implementing aforementioned the 1st~10 any scheme, can make with extra care more highly purified ammonia.

If adopt the ammonia refining device of the present invention's the 12nd scheme, after the distiller that heat exchanger constitutes imports thick ammonia gas, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, directly carry out the exhaust of gaseous phase by aforementioned exhaust channel from the aforementioned distiller lower-boiling impurity gas that boiling point is lower than ammonia, can from the aforementioned crude ammonia gas, remove lower-boiling impurity gas.

If adopt the refining plant of the present invention's the 13rd scheme, in aforementioned the 12nd scheme, establish at aforementioned distiller and to store the liquefied ammonia reservoir of liquefied ammonia, by using aforementioned heating unit that the liquefied ammonia in this liquefied ammonia reservoir is heated, can exhaust remove the lower-boiling impurity that residues in the liquefied ammonia, refining more highly purified ammonia.

If adopt the refining plant of the present invention's the 14th scheme, because after aforementioned liquefied ammonia reservoir discharge liquefied ammonia, use aforementioned gasification installation to make the liquefied ammonia gasification,, can supply with series-operation so the aforementioned the 12nd or 13 scheme can adopt gaseous phase to discharge high purity purified ammonia.

If adopt the refining plant of the present invention's the 15th scheme, can import thick ammonia gas in the water adsorption portion of adsorption moisture and the catalysing area of separated oxygen, from the aforementioned crude ammonia gas, remove moisture and oxygen at least as nonmetallic impurity.

If adopt the refining plant of the present invention's the 16th scheme, if the water adsorption portion of at least one pair of adsorption moisture and the catalysing area of separated oxygen, aforementioned water adsorption portion and aforementioned catalysing area a side import thick ammonia gas by aforementioned crude ammonia gas importing path, from the aforementioned crude ammonia gas, remove moisture and oxygen at least as nonmetallic impurity, regenerate by aforementioned reducing gas importing path feeding reducing gas at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area on the other hand, so can utilize the regeneration operation interruptedly not carry out the processing of removing of moisture and oxygen continuously, improve the purification efficiency of high purity ammonia.

If adopt the refining plant of the present invention's the 17th scheme, in aforementioned the 16th scheme, by utilizing aforementioned continuous treating control part control aforementioned crude ammonia gas to import the switch of path and aforementioned reducing gas importing path, can be to a pair of aforementioned water adsorption portion and each one of aforementioned catalysing area, alternately carry out the regeneration of removing and feeding aforementioned reducing gas of the moisture of aforementioned crude ammonia gas and oxygen repeatedly and make with extra care continuously, realize a large amount of refining of high purity ammonia.

If adopt the refining plant of the present invention's the 18th scheme, by aforementioned distiller, with be located at aforementioned distiller aforementioned lower-boiling impurity gas is directly carried out the aforementioned exhaust channel of gaseous phase deflated, to contain the thick ammonia gas liquefaction of moisture and the boiling point lower-boiling impurity gas lower than ammonia, can the exhaust that aforementioned lower-boiling impurity gas directly carries out gaseous phase be removed from aforementioned distiller, in addition, to use aforementioned gasification installation that the ammonia of liquefied ammonia gasification is imported aforementioned water adsorption portion and aforementioned catalysing area owing to import path by aforementioned ammonia, can from this ammonia, remove moisture and oxygen, therefore the continuous treatment process of impurity can be realized, more highly purified ammonia can be made with extra care.

If adopt the refining plant of the present invention's the 19th scheme, in aforementioned the 18th scheme, the liquefied ammonia reservoir of the ammonia that storage liquefied is set, by using aforementioned heating unit that the liquefied ammonia in this liquefied ammonia reservoir is heated, can separate and remove the lower-boiling impurity that residues in the liquefied ammonia, so can improve refining purity.

If adopt the refining plant of the present invention's the 20th scheme, in the aforementioned the 18th or 19 schemes, because aforementioned water adsorption portion and aforementioned catalysing area a side who establishes a pair of aforementioned water adsorption portion and aforementioned catalysing area at least import the ammonia that path imports aforementioned gasification installation gasification by aforementioned ammonia, from this ammonia, remove moisture and oxygen, aforementioned water adsorption portion and aforementioned catalysing area the opposing party are regenerated by aforementioned reducing gas importing path feeding reducing gas, therefore can with aforementioned water adsorption portion that utilizes a side and aforementioned catalysing area remove processing concurrently, carry out the opposing party's the aforementioned water adsorption portion and the manipulation of regeneration of aforementioned catalysing area, what can not interrupt adopting the regeneration operation removes operation and continuous treating.

If adopt the refining plant of the present invention's the 21st scheme, in aforementioned the 20th scheme, by utilizing aforementioned continuous treating control part control aforementioned crude ammonia gas to import the switch of path and aforementioned reducing gas importing path, can be to a pair of aforementioned water adsorption portion and each one of aforementioned catalysing area, alternately carry out the regeneration of removing and feeding aforementioned reducing gas of the moisture of aforementioned crude ammonia gas and oxygen repeatedly and make with extra care continuously, can realize a large amount of refining of high purity ammonia.

The 22nd scheme of the present invention, because the aforementioned crude ammonia gas is used raw material ammonia is separated into the gas phase composition gas that liquid phase and gas phase obtain, so utilize liquid phase to contain the character of moisture and metal species impurity in a large number, with the few vapor phase ammonia of moisture and metal species impurity part content as refining starting raw material, carry out refinement treatment by the process for purification of implementing aforementioned the 12nd~21 any scheme, can make with extra care more highly purified ammonia.

Description of drawings

Fig. 1 is the concise and to the point pie graph of refining plant of the present invention.

Fig. 2 is the concise and to the point pie graph of another refining plant of the present invention.

Fig. 3 is the concise and to the point pie graph of another refining plant of the present invention.

Fig. 4 is the ammonia consumption-gas phase moisture concentration distribution plan of the suitable ammonia user mode in the refining plant of explanatory view 3.

Embodiment

Below, the embodiment to ammonia process for purification of the present invention and refining plant at length describes with reference to the accompanying drawings.

According to Fig. 1 refining plant and the English process for purification of removing lower-boiling impurity from thick ammonia of the present invention described.Fig. 1 is the concise and to the point pie graph of the present embodiment refining plant.Raw material ammonia is contained in the ammonia liquor container 1, and the ammonia of its gas phase portion 12 becomes to be made with extra care uses thick ammonia.This raw material ammonia is separated into liquid phase portion 11 and gas phase portion 12, owing to this liquid phase, gas phase separation, so the moisture and the metal species impurity that are contained in the raw material ammonia remain in the liquid phase portion 11 basically.Therefore, the ammonia of the gas phase portion 12 that this liquid phase, gas phase separation obtain because moisture and metal species impurity become the state of removing in advance, so transfer to refining step in this state, as starting raw material ammonia, is to be suitable for the more refining raw material that uses of high purity.

Remove and be contained in the distillation tower 2 that the multiple nonmetallic impurity in the thick ammonia gas is used, distiller 3, gas inflow portion 7 that is located at pars intermedia that is made of the heat exchanger 31 that is located at this tower top and the liquefied ammonia reservoir 8 of being located at the bottom constitute.The heat exchanger 31 of distiller 3 is supplied with circulation road 41,42 by refrigerant and is connected coolant circulating device 4, and refrigerant is supplied with in heat exchanger 31 circulations.Refrigerant makes spent glycol etc., uses the temperature sensor monitors system (not diagram) that is located on the coolant circulating device 4, will remain on-5 ℃~+ 10 ℃ in the heat exchanger 31.Many gas passages 32 of heat exchanger 31 are communicated with formation between gas inflow portion 7 and distillation tower 2 topmost spaces 6.Gas inflow portion 7 is communicated with the gas phase portion 12 of ammonia liquor container 1 by gas supply passageway 9, by the thick ammonia gas of gas supply passageway 9 supplies from gas phase portion 12.Because the thick ammonia gas of supply gas inflow portion 7 enters gas passage 32, utilize the heat exchanger 31 and the cooling effect of coolant circulating device 4 to be liquefied, so fall at the liquefied ammonia reservoir 8 formation drops of distillation tower 2 foots, liquefied ammonia is stored.On the other hand, in topmost space 6, during the thick ammoniacal liquor of distiller 3, low-boiling foreign gas is piled up with a part of ammonia, by the exhaust channel 10 of being located at topmost space 6, utilize gas barrier (not having diagram) to carry out exhaust, so can discharge foreign gas.At this moment, the foreign gas that is deposited in topmost space 6 mainly is hydrogen (H 2), oxygen (O 2), carbon monoxide (CO), carbonic acid gas (CO 2), nitrogen (N 2), methane (CH 4) etc.

If adopt above-mentioned distiller 3, because with thick ammonia gas liquefaction, the limit makes liquefied ammonia 81 be stored in liquefied ammonia reservoir 8, the limit makes boiling point the contain nonmetallic impurity lower than ammonia separate as gas, therefore topmost space 6 can Separation and Recovery foreign gas, can once remove multiple impurity.So do not need the branch of the impurity of hydrogen, oxygen, carbon monoxide, carbonic acid gas, nitrogen, methane etc. is else removed operation, can adopt single distillation tower 2 simply and expeditiously to realize the high purifying of ammonia.

Distillation tower 2 also has the residual impurity degassing function of realizing the high purifying of ammonia.That is in, in the liquefied ammonia reservoir 8 if the warm water that warm water circulation device 5 is supplied with at the warm water circulation pipe arrangement 13 of reservoir internal recycle.The temperature sensor monitors system (there be not diagram) that warm water circulation device 5 is located in utilization remains on 30 ℃-50 ℃ with warm water, utilizes this warm water to circulate in warm water circulation pipe arrangement 13 surfaces and produces boiling (gasification).Therefore, remaining impurities is discharged to gas inflow portion 7 sides with after ammonia liquor is separated during thick ammoniacal liquor in the distiller 3, is recovered in topmost space 6 at last.

Because the heating function of the heating unit that utilizes above-mentioned warm water circulation device 5 and warm water circulation pipe arrangement 13 to constitute is composed sub-liquefied ammonia reservoir 8, therefore also can remove the impurity in the ammonia that residues in the portion's of being distilled 3 liquefaction, can further improve the refining purity of ammonia.

The ammonia liquor that is stored in liquefied ammonia reservoir 8 is discharged to gasification portion 15 sides by drain passageway 14.Gasification portion 15 is provided in the warm water tank 16.Establish well heater 18 in the warm water tank 16, utilize thermostatic control portion 17 to be controlled at 30 ℃~100 ℃ warm water state.Therefore, the ammonia liquor of discharging by drain passageway 14 is in gasification portion 15, is subjected to the pneumatolysis of the gasification installation that warm water tank 16 constitutes, and returns gaseous phase.Can utilize gas barrier (do not have diagram) ammonia behind this regasify refining to be discharged, obtain highly purified ammonia through gasification portion 15.

Below, describe removing the moisture that is contained in the thick ammonia and the refining plant and the process for purification thereof of oxygen efficiently according to Fig. 2.Fig. 2 is the concise and to the point pie graph of the present embodiment refining plant.The refining plant of the present embodiment is removed portion 20,21 by a pair of water, oxygen, carbon monoxide and is constituted.Water, oxygen, carbon monoxide are removed portion 20,21 and are had moisture respectively and remove portion 22 and remove portion 24 and catalysing area 25 with catalysing area 23, moisture.Moisture is removed the molecular sieve of the crystallinity zeolite composition of filling adsorption moisture in the portion 22,24.Moisture is removed portion 22,24 and is utilized the adsorption of molecular sieve to carry out removing of moisture.As moisture adsorbent, except molecular sieve, also can use the moisture adsorbent of activated alumina etc.Fill nickel catalyzator in the catalysing area 23,25.Utilize the chemisorption absorption of nickel catalyzator to remove deoxidation and carbon monoxide in the catalysing area 23,25.Utilize nickel catalyzator to remove deoxidation and carbon monoxide impurity is undertaken by following chemical reaction.

2Ni+O 2→2NiO

Ni+CO→Ni(CO)

Each water, oxygen, carbon monoxide are removed portion 20,21 and are formed 2 layers of isolating construction that moisture is removed portion and catalysing area.For example, make the refining amount of ammonia be 3N (standard state) m 3During/h, in the tube of internal diameter 43mm, fill molecular sieve 0.3kg (packing height: 300mm) in each moisture portion of removing.And, fill nickel catalyzator 0.8kg (packing height: 500mm) at each catalysing area.In addition, when the flow velocity of pressing 0.17m/s under the occupied state of these molecular sieves and nickel catalyzator feeds ammonia, remove with catalysing area, moisture that be about 3 seconds, 1.77 seconds the duration of contact of each sorbent material in the portion.In addition, water, oxygen, carbon monoxide are removed portion 20,21 make and make moisture adsorbent and the single composite construction of nickel catalyzator blended, also can obtain same adsorption effect.

Each water, oxygen, carbon monoxide are removed portion 20,21, import path 51 by thick ammonia gas, by importing path 29,30, import the gas phase ammonia from ammonia liquor container 50 respectively.Ammonia liquor container 50 be with Fig. 1 embodiment in the same structure of the ammonia liquor container that uses 1, raw material ammonia is carried out the few gas phase ammonia of moisture that liquid phase, gas phase separation obtain and metal species impurity as being used by processed gas.

In this device, refining step (bottom → top) is designed to reverse with the gas flow direction of step for regeneration (top → bottom).But step for regeneration also can similarly adopt bottom → top to carry out with refining step.The ammonia of portion 20,21 is removed in symbol 56,58,59 expressions towards water, oxygen, carbon monoxide gas imports the side switch-valve.In addition, the regeneration gas of the hydrogen reduction gas composition of being supplied with by regeneration gas feedway 54,55 imports path by regeneration gas, imports side switch-valve 61,64 by regeneration gas and supplies with each water, oxygen, carbon monoxide and remove portion 20,21.

Remove from each water, oxygen, carbon monoxide on the gas drain passageway 26,27 of portion 20,21 and be connected with exhaust channel 28, establish gas in addition on this gas drain passageway and discharge side switch-valve 62,63.In addition, be provided with from regeneration gas feedway 54,55 and feed regeneration gas, reclaim the regeneration gas retrieving arrangement 52,53 of this regeneration gas then to water, oxygen, the carbon monoxide portion of removing.The switch-valve 57,60 that configuration reclaiming gas is used on this recovery side path.

As regeneration gas, nickel catalyzator uses hydrogen with reducing gas, and the moisture of molecular sieve is removed the use drying nitrogen.Therefore feed hydrogen and nitrogen as regeneration gas.Each water, oxygen, the carbon monoxide portion of removing establish well heater 70,71, the heat treated when being used to regenerate.An example as manipulation of regeneration, at first, the limit is supplied with drying nitrogen by regeneration gas feedway 54 or 55 to water, oxygen, the carbon monoxide portion of removing, and carries out the removing 1 hour of moisture, and the limit is heated to about 200 ℃ with well heater 70,71 with water, oxygen, the carbon monoxide portion of removing.Then, under this heated condition, except supplying with the drying nitrogen from regeneration gas feedway 54 or 55, also hydrogen supply carries out the reduction of nickel catalyzator and handled 3 hours.The reduction of nickel catalyzator is handled and is undertaken by following chemical reaction.

NiO+H 2→Ni+H 2O

Ni(CO)+3H 2→Ni+CH 4+H 2O

Then, switch to and only supply with drying nitrogen, carry out remove 2 hours of adsorption moisture.At last, the limit feeds drying nitrogen, and the heating of well heater 70,71 was slowly reduced on the limit, approximately returned to normal temperature through 5 hours.In addition, the supply of regeneration gas for example makes the refining amount of ammonia be 3N (standard state) m 3During/h, be under 200N (standard state) L/h in dry nitrogen tolerance, also can make the reduction amounts of hydrogen is 4N (standard state) L/h.In addition, after manipulation of regeneration finishes, if do not transfer to immediately refining, the refining ammonia of the certain hour that before refining, circulates, then advantages of good adsorption effect.

Adopt above-mentioned formation, owing to use a pair of water, oxygen, carbon monoxide to remove portion 20,21, remove processing so a side is used for impurity, the opposing party then can carry out manipulation of regeneration.The refining management and control device of use (not diagram) for example, is opened gas from the state of closing whole valves and is imported side valve 56,58, opens the valve 62 of exhaust side again, and thick ammonia importing water, oxygen, carbon monoxide are removed portion 20.Because the importing of thick ammonia, utilize nickel catalyzator to remove deoxidation and carbon monoxide impurity at catalysing area 23, remove portion 22 at moisture again and utilize molecular sieve adsorption moisture to carry out removing of moisture impurity, remove continuously anhydrate, refining ammonia that oxygen and carbon monoxide obtain is discharged from by exhaust channel 28.

In addition, when water, oxygen, carbon monoxide are removed the refinement treatment end of portion's 20 sides, shut-off valve 58,62.Open valve 59,63 again, remove portion 21 to water, oxygen, carbon monoxide and import thick ammonia, useful catalyst portion 25 removes portion 24 with moisture and then carries out refinement treatment.On the other hand, water, oxygen, the carbon monoxide of finishing refinement treatment are removed portion 20, carry out above-mentioned manipulation of regeneration by opening valve 57,61.Like this,, regenerated refining by alternately each water, oxygen, the carbon monoxide portion of removing being switched to handled, and can utilize the impurity of water, oxygen to remove the continuous treating of realizing high purity ammonia gas, makes a large amount of refining possibilities that become.

Below, describe removing the refining plant and the process for purification thereof that are contained in the plurality of impurities in the thick ammonia expeditiously according to Fig. 3.Fig. 3 is the concise and to the point pie graph of the present embodiment refining plant.In addition, in the present embodiment, the structure identical with the embodiment of Fig. 1 and Fig. 2 used same-sign.

The refining plant of the present embodiment is removed portion 20,21 and is constituted by removing a pair of water, oxygen, the carbon monoxide that are contained in the distillation tower 2 that the multiple nonmetallic impurity in the thick ammonia gas uses and are used to remove moisture, oxygen and carbon monoxide impurity.Distillation tower 2 is removed portion 20,21 with water, oxygen, carbon monoxide, is respectively the structure same structure illustrated with Fig. 1, Fig. 2.In addition, the present embodiment also is at ammonia liquor container 1 raw material ammonia to be separated into liquid phase portion 11 and gas phase portion 12, with the vapor phase ammonia exhaust, imports distillation tower 2 as thick ammonia gas from this gas phase portion 12.The 19th, the switch-valve between gas phase portion 12 and gas supply passageway 9 and the gas inflow portion 7.

As previously mentioned, distillation tower 2 is made of distiller 3, the liquefied ammonia reservoir 8 being located at the gas inflow portion 7 of pars intermedia and being located at the bottom.Because lateral dominance liquefies thick ammonia gas with the liquefaction function of distiller 3, liquefied ammonia is stored in the liquefied ammonia reservoir 8, the limit nonmetallic impurity that contains that boiling point is lower than ammonia separates as gas, therefore can Separation and Recovery foreign gas in the topmost space 6 of distillation tower 2, can utilize exhaust once to remove multiple foreign gas G1 by exhaust channel 10.The foreign gas that is deposited in topmost space 6 mainly is hydrogen (H 2), oxygen (O 2), carbon monoxide (CO), carbonic acid gas (CO 2), nitrogen (N 2), methane (CH 4) etc.In addition, the heat effect of warm water circulation device 5 of the liquefied ammonia reservoir 8 of distillation tower 2 bottoms is located in utilization, in the distiller 3 during thick ammoniacal liquor remaining impurities also from ammonia liquor, separate, be discharged to gas inflow portion 7 sides, be recovered in topmost space 6 at last, can further improve refining purity.

The ammonia liquor that is stored in liquefied ammonia reservoir 8 is removed portion's 20,21 sides by drain passageway 14 through warm water tank 16 importing water, oxygen, carbon monoxide.Ammonia liquor is gasified once more by warm water tank 16, is imported water, oxygen, carbon monoxide as secondary by processed gas and removes portion's 20,21 sides.Each water, oxygen, carbon monoxide are removed portion 20,21 and are had moisture respectively and remove portion 22 and remove portion 24 and catalysing area 25 with catalysing area 23, moisture.Removing portion 22,24 at moisture utilizes the adsorption of the molecular sieve of being filled to carry out moisture to remove.Catalysing area 23,25 utilizes the chemisorption absorption of the nickel catalyzator of being filled to remove deoxidation and carbon monoxide.Therefore, remove portion 20,21 at each water, oxygen, carbon monoxide and can further remove and do not handle clean water, oxygen, carbon monoxide impurity in the distillation tower 2, adopt at last two steps by exhaust channel 28 removed in the plurality of impurities more, the highly purified refining ammonia G2 of water, oxygen and carbon monoxide impurity especially.

As mentioned above, the refining plant of the present embodiment is connected as refining system by distillation tower 2 and water, oxygen, carbon monoxide are removed portion 20,21, can realize simpler high purity refining step.In addition, as previously mentioned, alternately switch to refining, regeneration owing to use a pair of water, oxygen, carbon monoxide to remove portion 20,21, always can make a side carry out the refinement treatment running, the interruption of the refinement treatment in the time of therefore can avoiding making water, oxygen, carbon monoxide remove 20,21 o'clock regeneration of portion, but the continuous treating running is so help a large amount of purified cost degradations.

Table 1 expression embodies the impurities concentration distribution of above-mentioned refining plant refining effect and measures example.At first, the thick ammonia gas of gas phase portion 12 contains the hydrogen (H of ppm level concentration unit in a large number 2), oxygen (O 2), carbon monoxide (CO), carbonic acid gas (CO 2), nitrogen (N 2), methane (CH 4) lower-boiling impurity and the water (H that wait 2O) (with reference to (1) of table 1).When making with extra care this thick ammonia gas, shown in (3) of table 1, except water (H by distillation tower 2 2O) the most of impurity outside all reduce to the concentration unit of ppb level.In addition, owing to again processed gas importing water, oxygen, a carbon monoxide by distillation tower 2 are removed portion 20,21, so shown in (4) of table 1, water also reduces to the concentration unit of ppb level.Therefore, if adopt the process for purification that uses the present embodiment refining plant, can obtain the refining ammonia of extreme high purity.In addition, measure example, remove deoxidation, carbon monoxide impurity basically at distillation tower 2 according to this, few in the amount that water, oxygen, the carbon monoxide portion of removing removed in 20,21 stages.

In addition, initial because moisture is contained in the liquid phase in a large number, and the water in the vapor phase ammonia lacks than liquid phase shown in (2) of table 1, but when ammonia reduces gradually in the process of implementing continuous treating, produce the phenomenon that the moisture content in the gas phase sharply increases.The mensuration of the present embodiment refining plant is illustrated in Fig. 4.As seen from Figure 4, when the ammonia rate of utilization of ammonia liquor container 1 reached 85% left and right sides, the moisture in the gas phase increased sharp.Therefore, the normally refining limit of about 85% use as adopting the refining plant of the present embodiment, we can say that the continuous treating that reaches ammonia rate of utilization 85% is possible.

As mentioned above, adopt process for purification of the present invention and refining plant, can high purity the ground highly industry with raw material ammonia etc., and do not use complicated refining step, refining step can be oversimplified, and can form the continuous treating operation simply.

Table 1

Impurity Gas phase, the impurity component concentration unit of liquid phase: the v/vppm of thick ammonia Impurity component (3) after the use distillation tower refinement treatment Impurity component (4) concentration unit: v/vppb after refining final the processing Gas phase (1) Liquid phase (2) Concentration unit ????H 2 ?4 ??0.3 <50 ?v/vppb ??<50 ????O 2 ?20.6 ??0.2 <10 ?v/vppb ??<10 ????CO ?0.012 ??0.012 <10 ?v/vppb ??<10 ????CO 2 ?0.52 ??0.15 20 ?v/vppb ??<10 ????N 2 ?137.5 ??1.2 <10 ?v/vppb ??<10 ????CH 4 ?342 ??18.1 <10 ?v/vppb ??<10 ????H 2O ?13.8 ??1766 13.5 ?v/vppm ??<10

Claims (16)

1. ammonia refining method, it is that the thick ammonia gas that contains the boiling point lower-boiling impurity gas lower than ammonia is carried out the purified method, it is characterized in that, after being included in the distiller importing aforementioned crude ammonia gas of heat exchanger formation, utilize the cooling effect of aforesaid heat exchangers that ammonia is liquefied, from aforementioned distiller aforementioned lower-boiling impurity gas is directly carried out the exhaust of gaseous phase, from the aforementioned crude ammonia gas, remove first of aforementioned lower-boiling impurity gas and remove operation; Discharge the ammonia that liquefies at aforementioned distiller from aforementioned distiller, make it the gasification process that gasifies by the heating part; At least import the ammonia that gasifies in the aforementioned gasification process in water adsorption portion, dewatered second removes operation from this ammonia.
2. the described ammonia refining method of claim 1, it is characterized in that, at aforementioned distiller the liquefied ammonia reservoir of the ammonia that storage liquefied is set, by the liquefied ammonia in this liquefied ammonia reservoir is heated, the lower-boiling impurity that residues in the liquefied ammonia is removed in exhaust.
3. the described ammonia refining method of claim 2 is characterized in that, by discharging liquefied ammonia from aforementioned liquefied ammonia reservoir, makes it to gasify by the heating part.
4. the described ammonia refining method of claim 1 is characterized in that, removes in the operation aforementioned second, imports aforementioned ammonia at the catalysing area of separated oxygen, removes deoxidation from this ammonia.
5. the described ammonia refining method of claim 4, it is characterized in that, comprise that the 3rd removes operation, remove in the operation the described the 3rd, setting is stored in the aforementioned first liquefied ammonia reservoir of removing the ammonia that liquefies in the operation, the lower-boiling impurity that residues in the liquefied ammonia is removed in exhaust by the liquefied ammonia in this liquefied ammonia reservoir is heated, and removes operation by the aforementioned the 3rd and gasifies to aforementioned gasification process importing liquefied ammonia.
6. the described ammonia refining method of claim 4, it is characterized in that, aforementioned second removes operation comprises removing and handles and manipulation of regeneration, remove in the processing described, aforementioned water adsorption portion and aforementioned catalysing area a side who establishes a pair of aforementioned water adsorption portion and aforementioned catalysing area at least import the ammonia that aforementioned gasification process gasifies, from this ammonia, remove moisture and oxygen, in described manipulation of regeneration, regenerate at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area feeding reducing gas.
7. the described ammonia refining method of claim 6, it is characterized in that, to the aforementioned a pair of aforementioned water adsorption portion and the each several part of aforementioned catalysing area, alternately carry out the aforementioned aforementioned manipulation of regeneration of handling and feeding aforementioned reducing gas of removing of moisture and oxygen repeatedly, carry out continuous treating.
8. each described ammonia refining method of claim 1-7 is characterized in that, the aforementioned crude ammonia gas is raw material ammonia to be separated into liquid phase and gas phase and the gas phase composition gas that obtains.
9. ammonia refining device, it is that the thick ammonia gas that contains the boiling point lower-boiling impurity gas lower than ammonia is carried out the purified refining plant, it is characterized in that, after having the aforementioned crude of importing ammonia gas, utilize the distiller of cooling effect with the heat exchanger formation of ammonia liquefaction, the deflated exhaust channel that aforementioned lower-boiling impurity gas is directly carried out gaseous phase is set at aforementioned distiller, has the gasification installation that makes from the liquefied ammonia gasification of this distiller discharge, the water adsorption portion of adsorption moisture, at least the ammonia that imports aforementioned water adsorption portion with ammonia with the gasification of aforementioned gasification installation imports path, and the thick ammonia gas that contains moisture and aforementioned lower-boiling impurity gas is made with extra care.
10. the described ammonia refining device of claim 9 is characterized in that, the liquefied ammonia reservoir that aforementioned distiller comprises the thick ammonia of storing liquefaction be used for liquefied ammonia in the aforementioned liquefied ammonia reservoir and separate the heating unit of aforementioned lower-boiling impurity gas.
11. the described ammonia refining device of claim 10 is characterized in that, comprises the gasification installation that makes from the liquefied ammonia gasification of aforementioned distiller discharge.
12. the described ammonia refining device of claim 9 is characterized in that having the catalysing area of separated oxygen from aforementioned ammonia, aforementioned ammonia imports path by aforementioned ammonia and is imported into aforementioned catalysing area.
13. the described ammonia refining device of claim 12, it is characterized in that, the liquefied ammonia reservoir of the thick ammonia that is stored in aforementioned distiller liquefaction is located at aforementioned distiller, and aforementioned liquefied ammonia reservoir has the heating unit of the lower-boiling impurity that is used for the liquefied ammonia of separating residual in aforementioned liquefied ammonia reservoir.
14. the described ammonia refining device of claim 12, it is characterized in that, have at least one pair of aforementioned water adsorption portion and aforementioned catalysing area, the aforementioned ammonia that the ammonia that imports aforementioned gasification installation gasification is set at each aforementioned water adsorption portion and aforementioned catalysing area imports path, and the reducing gas importing path that imports reducing gas is set in each aforementioned water adsorption portion and aforementioned catalysing area, aforementioned water adsorption portion and aforementioned catalysing area a side import the ammonia that path imports aforementioned gasification by aforementioned ammonia, from this ammonia, remove moisture and oxygen, on the other hand, regenerate by aforementioned reducing gas importing path feeding reducing gas at the opposing party's aforementioned water adsorption portion and aforementioned catalysing area.
15. the described ammonia refining device of claim 14, it is characterized in that, continuous treating control part with switch of aforementioned ammonia importing path of control and aforementioned reducing gas importing path, make for the each several part of a pair of aforementioned water adsorption portion and aforementioned catalysing area, alternately carry out the regeneration of removing and feeding aforementioned reducing gas of the moisture and the oxygen of aforementioned crude ammonia gas repeatedly.
16. the described ammonia refining device of each of claim 9-15 is characterized in that, is provided with the separating and storing portion that raw material ammonia is separated into liquid phase and gas phase, the aforementioned crude ammonia gas is at the isolating gas phase composition gas of aforementioned separating and storing portion.
CNB2004100617629A 2003-12-03 2004-06-30 Refining method and device for ammonia CN1330573C (en)

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