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CN108358218A - A kind of ammonium hydroxide oil removing purification system and method - Google Patents

A kind of ammonium hydroxide oil removing purification system and method Download PDF

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Publication number
CN108358218A
CN108358218A CN201810064598.9A CN201810064598A CN108358218A CN 108358218 A CN108358218 A CN 108358218A CN 201810064598 A CN201810064598 A CN 201810064598A CN 108358218 A CN108358218 A CN 108358218A
Authority
CN
China
Prior art keywords
ammonia
ammonium hydroxide
oil
mixer
oil separator
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810064598.9A
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Chinese (zh)
Inventor
许开华
陈天斌
鲁旭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jingmen GEM New Material Co Ltd
Original Assignee
Jingmen GEM New Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jingmen GEM New Material Co Ltd filed Critical Jingmen GEM New Material Co Ltd
Priority to CN201810064598.9A priority Critical patent/CN108358218A/en
Publication of CN108358218A publication Critical patent/CN108358218A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/12Separation of ammonia from gases and vapours
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/022Preparation of aqueous ammonia solutions, i.e. ammonia water
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/024Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Degasification And Air Bubble Elimination (AREA)

Abstract

A kind of ammonium hydroxide oil removing purification system provided by the invention and method, include the gs-oil separator for detaching the organic phase in ammonia and the mixer for being mixed and being formed ammonium hydroxide with pure water to ammonia, the ammonia imports and ammonia outlet of the gs-oil separator are connected to form connection loop with the mixer respectively.System provided by the invention is to be connected to form loop with mixer by gs-oil separator, and liquid ammonia gasifier is equipped in mixer, part liquefied ammonia is gasificated into ammonia via liquid ammonia gasifier and enters oil removing separation in gs-oil separator, it is back to again in mixer and forms liquefied ammonia, ammonium hydroxide can recycle in this loop carries out oil removing separation, mixing, can greatly improve ammonium hydroxide oil removing dust removal rate.

Description

A kind of ammonium hydroxide oil removing purification system and method
Technical field
The present invention relates to ammonium hydroxide preparing technical field more particularly to a kind of ammonium hydroxide oil removing purification system and methods.
Background technology
Tertiary cathode material LixNiaCobMncO2Since self-discovery, because it (may be up to 250mAh/g, be with capacity height The 91% of theoretical capacity), the advantages that security performance is excellent and cheap, receive extensive concern and the research of people, and It has been obtained for being widely applied.Common multicomponent material such as stratiform cobalt acid lithium, spinel lithium manganate, LiFePO4, stratiform nickel Cobalt manganic acid lithium etc..Wherein, the polynary electrode material of stratiform nickle cobalt lithium manganate is that new type lithium ion battery developed in recent years is used Positive electrode, with relatively inexpensive nickel and manganese instead of the cobalt of higher price in cobalt acid lithium.Therefore, the compound is cost-effective Aspect has a clear superiority, meanwhile, reversible capacity is big, and stable structure has a safety feature, and has higher conductivity and heat steady It is qualitative, it is particularly suitable for making anode material for lithium-ion batteries.
And the impurity element of denier is mixed in common multicomponent material product, the resistivity of product will be made to occur very big Variation, influence safety and the chemical property of battery, thus polynary battery the degree of purity of chemical material is required it is high.
Ammonium hydroxide is the more common raw material arrived in polynary battery material production, and ammonia is usually used in preparation method and water is mixed It closes reaction to be made, but since TOC in common ammonia or other solid particulate matter impurity contents are high, in order to not influence production Obtained multicomponent material product quality, it is necessary to which clarification processing is carried out to the ammonium hydroxide being prepared.
Invention content
The present invention is to solve to exist in the prior artTOC contents or other solid particulate matter impurity contents are higher in ammonium hydroxide's Problem provides a kind of ammonium hydroxide oil removing purification system.
A kind of ammonium hydroxide oil removing purification system provided by the invention, includes the Oil-gas Separation for detaching the organic phase in ammonia Device and mixer for being mixed and being formed ammonium hydroxide with pure water to ammonia;The ammonia imports and ammonia of the gs-oil separator Outlet is connected to form connection loop with the mixer respectively.
Preferably, the gs-oil separator includes tank body, and the tank base is equipped with ammonia imports, its top is equipped with ammonia Outlet;It is equipped with the demister and partition board that the tank interior is separated into multiple chambers, institute in the tank body successively from the bottom to top It states in the chamber between demister and partition board filled with several ring-shaped articles for adsorbing organic matter.
Preferably, the ring-shaped article is stainless steel short tube section or ceramic ring.
Preferably, on the pipeline that the ammonia imports and ammonia outlet of the gs-oil separator are connected to the mixer respectively Equipped with control valve.
Preferably, liquid ammonia gasifier and ammonium hydroxide mixing chamber are equipped in the mixer, the liquid ammonia gasifier is equipped with liquefied ammonia Import and ammonia outlet, the ammonia outlet of the liquid ammonia gasifier are connected to the ammonia imports of the gs-oil separator, the oil The ammonia outlet of gas separating device is connected to the ammonium hydroxide mixing chamber.
Preferably, further include the Multistage filtering device that multistage filtering processing is carried out to ammonium hydroxide, the Multistage filtering device packet Include activated carbon oil expeller, coarse filter and the fine filter for passing sequentially through pipeline connection;The activated carbon oil expeller is mixed with described The liquefied ammonia outlet of clutch is connected to by pipeline;Pipeline between the activated carbon oil expeller and the mixer is equipped with iron remover And oil expeller.
The present invention also provides a kind of ammonium hydroxide oil removing purification process, the method is purified using ammonium hydroxide oil removing described above System includes the following steps:
S1:Gasification:The liquid ammonia material of entrance is gasificated into ammonia using liquid ammonia gasifier;
S2:Ammonia cleans:The ammonia, which is entered by liquid ammonia gasifier in gs-oil separator, to carry out for the first time except solid is outstanding Float and oil removal treatment;
S3:It is mixed with ammonium hydroxide:It is back in the ammonium hydroxide mixing chamber in mixer by the ammonias of step S2 after purification, gas Ammonia is mixed with pure water generates ammonium hydroxide;
S4:Multistage filtering purifies:The ammonium hydroxide obtained by step S3 carries out second except solid by oil expeller and iron remover Body suspended matter and oil removal treatment;Ammonium hydroxide by second of removal of impurities processing, which respectively enters, carries out essence in coarse filter and fine filter Refinement filtering.
Preferably, the filtering accuracy of the coarse filter is 0.5 μm, and the filtering accuracy of the fine filter is 0.1 μm.
Preferably, the pressure in the gs-oil separator is 0~1.6MPa;Pressure in the coarse filter and fine filter Power is respectively 0~0.25MPa.
Beneficial effects of the present invention are mainly as follows:
(1) by liquid ammonia gasification at gaseous state, the separating degree between ammonia and oil and solid impurity not only can be improved, can also increase With the contact area of cyclic annular adsorption piece in gs-oil separator, oil and impurity in ammonium hydroxide can be effectively reduced.
(2) gs-oil separator is connected to form loop with mixer, and liquid ammonia gasifier is equipped in mixer, part liquefied ammonia warp Ammonia is gasificated by liquid ammonia gasifier and enters oil removing separation in gs-oil separator, then is back in mixer and forms ammonium hydroxide, it can pole The earth improves ammonium hydroxide oil removing dust removal rate.
(3) purification system of the invention carries out ammonium hydroxide by gs-oil separator, activated carbon oil expeller, Multistage filtering device Multistep oil removing edulcoration purification, TOC contents are reduced to 40mg/L or less in finally obtained ammonium hydroxide.
Description of the drawings
Fig. 1 is a kind of ammonium hydroxide oil removing purification system structure chart of the embodiment of the present invention;
Fig. 2 is the structure chart of gs-oil separator in Fig. 1.
Reference sign:
1- gs-oil separators;The ammonia of the ammonia 1b- gs-oil separators of 1a- gs-oil separators
Import;Outlet;
2- mixers;3- activated carbon oil expellers;4- coarse filters;
5- fine filters;11- demisters;12- partition boards;
13- ring-shaped articles;14- control valves;21- liquid ammonia gasifiers;
The ammonia 22- ammonium hydroxide mixing chambers of the liquid 21b- liquid ammonia gasifiers of 21a- liquid ammonia gasifiers.
Ammonia import;Gas exports;
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below Example is not limited to the scope of the present invention for illustrating the present invention.
A kind of ammonium hydroxide oil removing purification system of the embodiment of the present invention includes for detaching the oil gas of the organic phase in ammonia point Mixer 2 from device 1, for being mixed and being formed ammonium hydroxide with pure water to ammonia and multistage filtering processing is carried out to ammonium hydroxide Multistage filtering device.
Specifically, the ammonia imports 1a and ammonia outlet 1b of the gs-oil separator 1 are connected to shape with the mixer 1 respectively At connection loop.Gs-oil separator 1 is connected to form loop with mixer 2, and liquid ammonia gasifier 21, part are equipped in mixer 2 Liquefied ammonia is gasificated into ammonia via liquid ammonia gasifier 21 and enters oil removing separation in gs-oil separator, then is back in mixer and forms ammonia Water can greatly improve ammonium hydroxide oil removing dust removal rate.Heating ammonium hydroxide is can be used into the method that liquefied ammonia gasifies or in container Pressure or decompression obtain ammonia.
Specifically, the gs-oil separator 1 includes tank body, and the tank base is equipped with ammonia imports, its top is equipped with ammonia Gas exports;It is equipped with the demister 11 and partition board that the tank interior is separated into multiple chambers in the tank body successively from the bottom to top 12, the chamber between the demister 11 and partition board 12 is interior filled with several ring-shaped articles 13 for adsorbing organic matter.Liquefied ammonia gas More solid suspension is will produce during chemical conversion ammonia, demister 11 can remove the solid impurity in ammonia, by removing Miscellaneous ammonia enters in split cavity, and the oil in ammonia is carried out adsorbing separation by the ring-shaped article 13 with suction-operated, The ring-shaped article 13 can be stainless steel short tube section or ceramic ring, and stainless steel and ceramic material have certain condensation to imitate organic phase oil Fruit, organic phase oil can coagulate on short tube section or ceramic ring surface, oil detached with ammonia, with common acticarbon phase Not only adhere to that oil effect is good than, stainless steel short tube section or ceramic ring, and the amount of ammonia will not be lost, it will not be additionally into ammonia Bring new impurity into, since stainless steel and ceramic material surface roughness are small, after oil is saved bit by bit to a certain degree, the attachment of oil Power is reduced and is detached from 13 surface of ring-shaped article, therefore oil removing can be repeated without influencing oil removing effect in stainless steel short tube section or ceramic ring Rate, usage time are long.
The pipe that can be connected to respectively with the mixer 2 in the ammonia imports 1a and ammonia outlet 1b of the gs-oil separator 1 Road is equipped with control valve 14, can control the input of ammonia and the output of liquefied ammonia.
Based on above-described embodiment, in the present embodiment, liquid ammonia gasifier 21 and ammonium hydroxide mixing chamber are equipped in the mixer 2 22, the ammonia outlet 21b of the liquid ammonia gasifier 21 is connected to the ammonia imports 1a of the gs-oil separator 1, the oil gas point Ammonia outlet 1b from device 1 is connected to the ammonium hydroxide mixing chamber 22;Liquefied ammonia enters from the feed inlet of mixer 2 in mixer 2, portion Liquid separation ammonia, which is entered by the liquefied ammonia import 21a of liquid ammonia gasifier 21 in liquid ammonia gasifier 21, to gasify, and divides subsequently into gs-oil separator 1 From isolated pure ammonia flows back into mixer 2, is mixed with pure water and generates ammonium hydroxide, mixer 2 and Oil-gas Separation The connection of device 1 forming circuit greatly improves the removal efficiency of the oil and impurity in ammonium hydroxide, it can be achieved that oil removing purifying.
Based on above-described embodiment, in the present embodiment, the Multistage filtering device includes the activity for passing sequentially through pipeline connection Charcoal oil expeller 3, coarse filter 4 and fine filter 5;The activated carbon oil expeller 3 and the liquefied ammonia outlet of the mixer 2 pass through pipe Road is connected to;Pipeline between the activated carbon oil expeller 3 and the mixer 2 is equipped with iron remover 4 and oil expeller 5.Multistage mistake Filter device can further remove the smaller impurity of particle rank, and ammonium hydroxide is further purified.
Based on the ammonium hydroxide oil removing purification system that above-described embodiment provides, a kind of ammonium hydroxide oil removing provided in an embodiment of the present invention is pure Change method, the described method comprises the following steps:
S1:Gasification:The liquid ammonia material of entrance is gasificated into ammonia using liquid ammonia gasifier;
S2:Ammonia cleans:The ammonia, which is entered by liquid ammonia gasifier in gs-oil separator, to carry out for the first time except solid is outstanding Float and oil removal treatment;
S3:It is mixed with ammonium hydroxide:It is back in the ammonium hydroxide mixing chamber in mixer by the ammonias of step S2 after purification, ammonia Gas is mixed with pure water generates ammonium hydroxide;
S4:Multistage filtering purifies:The ammonium hydroxide obtained by step S3 carries out second except solid by oil expeller and iron remover Body suspended matter and oil removal treatment;Ammonium hydroxide by second of removal of impurities processing, which respectively enters, carries out essence in coarse filter and fine filter Refinement filtering.
The filtering accuracy of the coarse filter is 0.5 μm, and the filtering accuracy of the fine filter is 0.1 μm.Coarse filtration is smart again Filter, can further remove the Solid content and oil in ammonium hydroxide, can also remove the smaller granule foreign of grain size rank, improve ammonium hydroxide Purity.
Pressure in the gs-oil separator is 0~1.6MPa;Pressure difference in the coarse filter and fine filter For 0~0.25MPa.Smaller pressure is used in container, the upward flow velocity of ammonia can be improved, to improve separative efficiency.
Finally, method of the invention is only preferable embodiment, is not intended to limit the scope of the present invention.It is all Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the protection of the present invention Within the scope of.

Claims (9)

1. a kind of ammonium hydroxide oil removing purification system, it is characterised in that:It include the gs-oil separator for detaching the organic phase in ammonia With the mixer for being mixed and being formed ammonium hydroxide with pure water to ammonia;
The ammonia imports and ammonia outlet of the gs-oil separator are connected to form connection loop with the mixer respectively.
2. ammonium hydroxide oil removing purification system as described in claim 1, it is characterised in that:The gs-oil separator includes tank body, institute It states tank base and is equipped with ammonia outlet equipped with ammonia imports, its top;It is equipped with successively by the tank from the bottom to top in the tank body Internal body portion is divided into the demister and partition board of multiple chambers, is used for filled with several in the chamber between the demister and partition board Adsorb the ring-shaped article of organic matter.
3. ammonium hydroxide oil removing purification system as claimed in claim 2, it is characterised in that:The ring-shaped article be stainless steel short tube section or Ceramic ring.
4. ammonium hydroxide oil removing purification system as claimed in claim 2, it is characterised in that:The ammonia imports of the gs-oil separator and The pipeline that ammonia outlet is connected to the mixer respectively is equipped with control valve.
5. ammonium hydroxide oil removing purification system as described in claim 1, it is characterised in that:Liquid ammonia gasifier is equipped in the mixer With ammonium hydroxide mixing chamber, the liquid ammonia gasifier be equipped with liquefied ammonia import and ammonia outlet, the ammonia outlet of the liquid ammonia gasifier with The ammonia imports of the gs-oil separator are connected to, and the ammonia outlet of the gs-oil separator is connected to the ammonium hydroxide mixing chamber.
6. ammonium hydroxide oil removing purification system as described in claim 1, it is characterised in that:Further include being carried out at multistage filtering to ammonium hydroxide The Multistage filtering device of reason, the Multistage filtering device include the activated carbon oil expeller for passing sequentially through pipeline connection, coarse filter And fine filter;The activated carbon oil expeller is exported with the liquefied ammonia of the mixer and is connected to by pipeline;The activated carbon oil removing Pipeline between device and the mixer is equipped with iron remover and oil expeller.
7. a kind of ammonium hydroxide oil removing purification process, it is characterised in that:The method is removed using the ammonium hydroxide as described in claim 1~6 Oily purification system, includes the following steps:
S1:Gasification:The liquid ammonia material of entrance is gasificated into ammonia using liquid ammonia gasifier;
S2:Ammonia cleans:The ammonia, which is entered by liquid ammonia gasifier in gs-oil separator, to carry out removing solid suspension for the first time And oil removal treatment;
S3:It is mixed with ammonium hydroxide:The ammonium hydroxide mixing chamber being back to by pipeline by the ammonias of step S2 after purification in mixer In, ammonia is mixed with pure water generates ammonium hydroxide;
S4:Multistage filtering purifies:The ammonium hydroxide obtained by step S3 carries out second except solid is outstanding by oil expeller and iron remover Float and oil removal treatment;Ammonium hydroxide by second of removal of impurities processing, which respectively enters in coarse filter and fine filter, to be refined Filtering.
8. ammonium hydroxide preparation and purification method as claimed in claim 7, it is characterised in that:The filtering accuracy of the coarse filter is 0.5 μm, the filtering accuracy of the fine filter is 0.1 μm.
9. ammonium hydroxide preparation and purification method as claimed in claim 7, it is characterised in that:Pressure in the gs-oil separator is 0~1.6MPa;Pressure in the coarse filter and fine filter is respectively 0~0.25MPa.
CN201810064598.9A 2018-01-23 2018-01-23 A kind of ammonium hydroxide oil removing purification system and method Pending CN108358218A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810064598.9A CN108358218A (en) 2018-01-23 2018-01-23 A kind of ammonium hydroxide oil removing purification system and method

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Application Number Priority Date Filing Date Title
CN201810064598.9A CN108358218A (en) 2018-01-23 2018-01-23 A kind of ammonium hydroxide oil removing purification system and method

Publications (1)

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CN108358218A true CN108358218A (en) 2018-08-03

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030108473A1 (en) * 2000-12-27 2003-06-12 Ashland Inc. Process for producing ammonia with ultra-low metals content
CN201959660U (en) * 2011-01-21 2011-09-07 西安同大实业有限公司 High-efficient ammonia oil removal filter
CN103880039A (en) * 2012-12-19 2014-06-25 海安海太铸造有限公司 Ammonia purifying and deoiling device
CN104743575A (en) * 2015-03-19 2015-07-01 苏州晶瑞化学有限公司 Continuous production method of high-purity ammonia water
CN204582611U (en) * 2015-04-21 2015-08-26 齐炜 A kind of liquefied ammonia (ammonia) is dewatered oil removal filter
JP2016188154A (en) * 2015-03-30 2016-11-04 大陽日酸株式会社 Method for purifying ammonia

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030108473A1 (en) * 2000-12-27 2003-06-12 Ashland Inc. Process for producing ammonia with ultra-low metals content
CN201959660U (en) * 2011-01-21 2011-09-07 西安同大实业有限公司 High-efficient ammonia oil removal filter
CN103880039A (en) * 2012-12-19 2014-06-25 海安海太铸造有限公司 Ammonia purifying and deoiling device
CN104743575A (en) * 2015-03-19 2015-07-01 苏州晶瑞化学有限公司 Continuous production method of high-purity ammonia water
JP2016188154A (en) * 2015-03-30 2016-11-04 大陽日酸株式会社 Method for purifying ammonia
CN204582611U (en) * 2015-04-21 2015-08-26 齐炜 A kind of liquefied ammonia (ammonia) is dewatered oil removal filter

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
黄亚东等: "《化工原理》", 30 September 2006, 北京:中国轻工业出版社 *

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Application publication date: 20180803

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