CN110002474A - Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product - Google Patents
Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product Download PDFInfo
- Publication number
- CN110002474A CN110002474A CN201910370843.3A CN201910370843A CN110002474A CN 110002474 A CN110002474 A CN 110002474A CN 201910370843 A CN201910370843 A CN 201910370843A CN 110002474 A CN110002474 A CN 110002474A
- Authority
- CN
- China
- Prior art keywords
- potassium
- salt solution
- ammonium salt
- potassium nitrate
- crude product
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/16—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the Ammonia recovery techniques containing ammonium salt solution after a kind of purification of potassium nitrate crude product, comprising the following steps: (1) containing the preparation of ammonium salt solution；(2) ammonium is removed containing ammonium salt solution；(3) spray recycling；(4) condensing recovery.The invention can avoid the pollution of ammonia direct emission, the recycling ammonias of energy 100%, and the product of Ammonia recovery can be recycling in the process of preparing potassium nitrate by means of double decomposition and byproduct ammonium chloride, improved the utilization rate of resource, reduced production cost.
Description
Technical field
The present invention relates to a kind of Ammonia recovery technique, in particular to the ammonia containing ammonium salt solution after a kind of potassium nitrate crude product purification
Recovery process.
Background technique
Potassium nitrate also known as nitre, sal prunella, nitre, chemical formula KNO3, it is a kind of no chlorine High-quality fertilizer and inorganic chemical industry
Product is industrially widely used in agricultural and.Agriculturally, potassium nitrate is especially suitable as a kind of good chlorideless potassic fertilizer
The nonirrigated farmland industrial crops of chlorine happiness potassium are avoided for tobacco, coffee, tealeaves, flowers etc., and potassium nitrate is by effective substance as fertilizer
Matter composition, will not change soil quality or cause crop lesion after application；Industrially, potassium nitrate is mainly for the manufacture of gunpowder, gold
Belong to welding auxiliary agent, synthetic ammonia catalyst, glassware, ceramics etc.；It can be used as colour former, the preservative of meat products in terms of food
Deng；Medical aspect also acts as diuretics, freshener and produces the drugs such as potassium salt of penicillin, rifampin.In addition, technical grade nitre
Sour potassium also presents good development prospect using upper in terms of glass manufacture in recent years, and the U.S. just has begun nitre in the early time
Sour potassium is used for the manufacture of optical glass, and many glass producers also start in succession using Production of Potassium Nitrate mobile phone screen and plate now
The high-end chemically reinforced glass such as computer, as China's economic continues, stable development, the development space of potassium nitrate will be increasingly
Greatly, the market demand can be also constantly increasing.Currently, both at home and abroad production potassium nitrate main technique have conversion method, ion-exchange,
Solvent extraction and double decomposition, wherein double decomposition is the major processes of domestic product potassium nitrate.
Using inevitably there are ammonium chloride impurities in potassium nitrate crude product made from potassium chloride-ammonium nitrate double decomposition.
Chinese patent CN105060317A discloses " a kind of to produce high-quality potassium nitrate by potassium chloride and ammonium nitrate double decomposition circulation process
Method ", this method is using potassium chloride and ammonium nitrate as raw material, including raw material preparation, potassium nitrate crystal, froth flotation separation, nitric acid
The technical process such as potassium purification and ammonium chloride crystals.The present invention is the improvement to traditional Production of Potassium Nitrate some processes, wherein foam
Floatation separation process is in the presence of C12~C20 high straight chain fatty amine floating agent and within the scope of certain pH value by gas
The form for acting through foam entrainment of bubble is naturally completed the separation of ammonium chloride Yu crude product potassium nitrate, the subtractive process of potassium nitrate
It is to first pass through the smart potassium mother liquor rinsing crude product potassium nitrate that one recycles to realize through operations such as sodium carbonate purifications again.On the one hand, excellent
Change traditional process for producing potassium nitrate, improved the quality of potassium nitrate, considerably reduces the impurity content of potassium nitrate product；Separately
On the one hand, the usage amount for reducing water, reduces labor intensity, has saved production cost.It is in this method that crude product potassium nitrate is molten
Potassium carbonate is accessed after solution, ammonium chloride and carbonic acid nak response generate ammonia to remove the NH in crude product potassium nitrate solution4 +, and ammonia is made
It discharges pollutants for national legislation limit value, in this method and the recycling of unresolved ammonia.
Summary of the invention
The purpose of the present invention is making improvements and innovating for shortcoming and defect present in background technique, a kind of nitre is provided
Ammonia recovery technique containing ammonium salt solution after sour potassium crude product purification, the Ammonia recovery technique are avoided that the pollution of ammonia direct emission,
The recycling ammonia of energy 100%, and the product of Ammonia recovery can be recycling in preparing potassium nitrate by means of double decomposition and byproduct chlorine
In the process for changing ammonium, the utilization rate of resource is improved, production cost is reduced.
To achieve the above object, the technical solution adopted by the present invention is that: containing ammonium salt solution after a kind of purification of potassium nitrate crude product
Ammonia recovery technique, comprising the following steps:
(1) containing the preparation of ammonium salt solution: pure water rinses potassium nitrate crude product, up to the mass fraction of ammonium chloride in potassium nitrate crude product
It is 0.3~0.5%, then the pure water after use is then containing ammonium salt solution；
There are ammonium chloride impurities in the potassium nitrate crude product as made from potassium chloride-ammonium nitrate double decomposition, in rinsing, nitre
Ammonium chloride, part potassium nitrate in sour potassium crude product are dissolved in pure water, become pure water containing ammonium salt solution, the pure water after rinsing then contains
Potassium nitrate, ammonium chloride and potassium chloride.
(2) ammonium being removed containing ammonium salt solution: containing ammonium salt solution and be passed through in reaction kettle, sylvite is added and is heated to reacting, reaction is made
Ammonia and potassium salt soln；
By containing mixing in ammonium salt solution with sylvite, which selects one of potassium carbonate, potassium hydroxide, and using containing, ammonium is molten
Ammonium chloride in liquid reacts under conditions of 100 DEG C with sylvite, generates ammonia and potassium chloride, and ammonia is passed through in spray column through collecting
It handles, the potassium nitrate in the potassium chloride and original solution of generation becomes potassium salt soln jointly.Again by potassium salt soln crystallisation by cooling, it is precipitated
Potassium nitrate, potassium chloride, after being separated by solid-liquid separation, potassium nitrate, the potassium chloride isolated are recycling in potassium chloride-nitre
In the process of sour ammonium preparing potassium nitrate by means of double decomposition, remaining solution is followed as the pure water in rinsing mother liquor alternative steps (1)
Ring uses.
The reaction equation of potassium carbonate and ammonium chloride:
The reaction equation of potassium hydroxide and ammonium chloride:
(3) spray recycling: the ammonia in step (2) is passed through in spray column, is sprayed and is inhaled with the dust technology that concentration is 20%
It receives, ammonium nitrate solution and tail gas is made；
Ammonia is passed through in spray column and is absorbed with removing ammonia agent, should be except the dust technology that ammonia agent is concentration 20%, dust technology and big
Ammonium nitrate solution is generated after the ammonia reaction of amount, and when ammonium nitrate solution pH value is 5~6, ammonium nitrate solution can recycle benefit
The preparation of byproduct ammonium chloride for double decomposition legal system potassium nitrate.But the dust technology in spray column cannot inhale completely ammonia
It receives, and dust technology reacts with ammonia and belongs to exothermic reaction, releasing heat can be generated generates a small amount of vapor in spray column, because
Also contain a small amount of ammonia and vapor in the tail gas of this spray column discharge.
The reaction equation of dust technology and ammonia:
HNO3+NH3=NH4NO3
(4) condensing recovery: the tail gas after spray-absorption in step (3) is passed through in condensing heat exchanger, and condensed water, institute is made
State the rinsing that condensate water circulatory is used in the byproduct ammonium chloride of double decomposition legal system potassium nitrate.
It can be recycled completely after being condensed into condensed water due to containing a small amount of ammonia and vapor in tail gas
Ammonia.And condensed water can also be recycling in the rinsing of the byproduct ammonium chloride of double decomposition legal system potassium nitrate.
Preferably, sylvite is one of potassium carbonate, potassium hydroxide in the step (2), and the heating temperature is 100
℃。
Preferably, the sylvite is potassium carbonate, described to contain ammonium salt solution and potassium carbonate K in molar ratio2CO3: NH4Cl=1:2 is mixed
It closes.
Preferably, the sylvite is potassium hydroxide, described to contain ammonium salt solution and potassium hydroxide KOH:NH in molar ratio4Cl=1:
1 mixing.
Preferably, when ammonium nitrate solution pH value described in the step (3) is 5~6, the ammonium nitrate solution is recycled
In the preparation of the byproduct ammonium chloride of double decomposition legal system potassium nitrate.
Advantages of the present invention and the utility model has the advantages that
The present invention obtains passing through potassium carbonate or hydrogen containing ammonium salt solution using ammonium chloride in pure water rinsing removal potassium nitrate crude product
Potassium oxide react with containing ammonium salt solution except ammonium, generates ammonia and potassium chloride, and ammonia is handled through collecting to be passed through in spray column, potassium chloride and
Potassium nitrate in original solution becomes potassium salt soln jointly.Again by potassium salt soln crystallisation by cooling, potassium nitrate, potassium chloride is precipitated,
After being separated by solid-liquid separation, potassium nitrate, the potassium chloride isolated are recycling in potassium chloride-ammonium nitrate double decomposition production nitre
In the process of sour potassium, pure water of the remaining solution as rinsing mother liquor substitution potassium nitrate crude product, and be recycled.Ammonia is passed through spray
It drenching in tower and absorbs ammonia with the dilute nitric acid reaction of concentration 20%, dust technology generates ammonium nitrate solution after reacting with a large amount of ammonia,
And when ammonium nitrate solution pH value is 5~6, ammonium nitrate solution be can be recycled in the byproduct chlorination of double decomposition legal system potassium nitrate
The preparation of ammonium.The tail gas of spray column discharge is condensed into condensed water by condensing heat exchanger, just recycles ammonia, Er Qieleng completely
Condensate can also be recycling in the rinsing of the byproduct ammonium chloride of double decomposition legal system potassium nitrate.This avoids ammonia direct emissions
Pollution, realizes 100% recycling ammonia, and the product of Ammonia recovery can be recycling in preparing potassium nitrate by means of double decomposition and
In the process of byproduct ammonium chloride, the utilization rate of resource is improved, production cost is reduced.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product, comprising the following steps:
(1) containing the preparation of ammonium salt solution: potassium nitrate crude product is rinsed with pure water, until the quality of ammonium chloride is divided in potassium nitrate crude product
Number is 0.3~0.5%, then the pure water after use is then to contain containing ammonium salt solution and contain potassium nitrate, ammonium chloride and chlorination in ammonium salt solution
Potassium.
(2) ammonium is removed containing ammonium salt solution: will contain ammonium salt solution and be passed through in reaction kettle, in molar ratio K2CO3: NH4Carbon is added in Cl=1:2
Sour potassium is reacted with containing the ammonium chloride in ammonium salt solution, while being heated to 100 DEG C, reacts and ammonia and potassium salt soln is made；Potassium salt soln
In contain potassium nitrate, potassium chloride.
The reaction equation of potassium carbonate and ammonium chloride:
(3) spray recycling: the ammonia in step (2) is passed through in spray column, is sprayed and is inhaled with the dust technology that concentration is 20%
It receives, ammonium nitrate solution and tail gas is made；When ammonium nitrate solution pH value is 5, which is recycling in double decomposition
The preparation of the byproduct ammonium chloride of potassium nitrate processed, and contain a small amount of ammonia and vapor in tail gas.
The reaction equation of dust technology and ammonia:
HNO3+NH3=NH4NO3
(4) condensing recovery: the tail gas after spray-absorption in step (3) is passed through in condensing heat exchanger, and condensed water, institute is made
State the rinsing that condensate water circulatory is used in the byproduct ammonium chloride of double decomposition legal system potassium nitrate.
Embodiment 2
Unlike the first embodiment:
In step (2), ammonium salt solution will be contained and be passed through in reaction kettle, in molar ratio KOH:NH4Cl=1:1 be added potassium hydroxide with
Containing the ammonium chloride reaction in ammonium salt solution, while 100 DEG C are heated to, react and ammonia and potassium salt soln is made；Contain in potassium salt soln
Potassium nitrate, potassium chloride.
The reaction equation of potassium hydroxide and ammonium chloride:
In step (3), when ammonium nitrate solution pH value is 5, which is recycling in double decomposition legal system nitric acid
The preparation of the byproduct ammonium chloride of potassium.
Remaining content is same as Example 1.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field
Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within
Within protection scope of the present invention.
Claims (5)
1. the Ammonia recovery technique containing ammonium salt solution after a kind of potassium nitrate crude product purification, it is characterised in that following steps:
(1) containing the preparation of ammonium salt solution: pure water rinses potassium nitrate crude product, until the mass fraction of ammonium chloride is in potassium nitrate crude product
0.3~0.5%, then the pure water after use is then containing ammonium salt solution；
(2) ammonium is removed containing ammonium salt solution: will contain ammonium salt solution and be passed through in reaction kettle, sylvite is added and is heated to reacting, react and ammonia is made
And potassium salt soln；
(3) spray recycling: the ammonia in step (2) is passed through in spray column, the dust technology spray-absorption for being 20% with concentration, system
Obtain ammonium nitrate solution and tail gas；
(4) condensing recovery: the tail gas after spray-absorption in step (3) is passed through in condensing heat exchanger, and condensed water is made, described cold
Condensate is recycling in the rinsing of the byproduct ammonium chloride of double decomposition legal system potassium nitrate.
2. the Ammonia recovery technique containing ammonium salt solution after a kind of potassium nitrate crude product purification according to claim 1, feature exist
Sylvite is one of potassium carbonate, potassium hydroxide in the step (2), and the heating temperature is 100 DEG C.
3. the Ammonia recovery technique containing ammonium salt solution after a kind of potassium nitrate crude product purification according to claim 2, feature exist
In the sylvite be potassium carbonate, it is described containing ammonium salt solution and potassium carbonate K in molar ratio2CO3: NH4Cl=1:2 mixing.
4. the Ammonia recovery technique containing ammonium salt solution after a kind of potassium nitrate crude product purification according to claim 2, feature exist
In the sylvite be potassium hydroxide, it is described containing ammonium salt solution and potassium hydroxide KOH:NH in molar ratio4Cl=1:1 mixing.
5. the Ammonia recovery technique containing ammonium salt solution after a kind of potassium nitrate crude product purification according to claim 1, feature exist
When the ammonium nitrate solution pH value described in the step (3) is 5~6, which is recycling in double decomposition legal system nitre
The preparation of the byproduct ammonium chloride of sour potassium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910370843.3A CN110002474A (en) | 2019-05-06 | 2019-05-06 | Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910370843.3A CN110002474A (en) | 2019-05-06 | 2019-05-06 | Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110002474A true CN110002474A (en) | 2019-07-12 |
Family
ID=67175779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910370843.3A Pending CN110002474A (en) | 2019-05-06 | 2019-05-06 | Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110002474A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB382372A (en) * | 1930-09-11 | 1932-10-27 | Jacob Manne Elgersma | Improved extraction process for obtaining substances in purified condition |
| CN105480988A (en) * | 2015-12-15 | 2016-04-13 | 赣州逸豪优美科实业有限公司 | Method for preparing high-purity ammonium salts from high-impurity ammonium salt waste liquor |
| JP2016087573A (en) * | 2014-11-07 | 2016-05-23 | 栗田工業株式会社 | Water recovery device and electrodialyzer |
| CN107162022A (en) * | 2017-05-28 | 2017-09-15 | 赵家春 | Production of Potassium Nitrate method |
| CN107758960A (en) * | 2017-10-18 | 2018-03-06 | 江苏理工学院 | A kind of processing method of ammonia waste water |
-
2019
- 2019-05-06 CN CN201910370843.3A patent/CN110002474A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB382372A (en) * | 1930-09-11 | 1932-10-27 | Jacob Manne Elgersma | Improved extraction process for obtaining substances in purified condition |
| JP2016087573A (en) * | 2014-11-07 | 2016-05-23 | 栗田工業株式会社 | Water recovery device and electrodialyzer |
| CN105480988A (en) * | 2015-12-15 | 2016-04-13 | 赣州逸豪优美科实业有限公司 | Method for preparing high-purity ammonium salts from high-impurity ammonium salt waste liquor |
| CN107162022A (en) * | 2017-05-28 | 2017-09-15 | 赵家春 | Production of Potassium Nitrate method |
| CN107758960A (en) * | 2017-10-18 | 2018-03-06 | 江苏理工学院 | A kind of processing method of ammonia waste water |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101746822B (en) | Method for extracting sodium metavanadate from vanadium extraction leaching solution | |
| CN101219974B (en) | Method for recovery utilization of mother solution hydrochloric acid for ADC foaming agent production | |
| CN102502708B (en) | Preparation method for preparing alkali metal or alkali earth metal cyanide with high purity and high yield | |
| CN109052434B (en) | Method for jointly producing soda ash and composite nitrogen fertilizer by taking mirabilite and ammonium bicarbonate as raw materials | |
| CN103818933A (en) | Method for production of high-purity potassium fluoride by using hydrofluoric acid residual liquid | |
| CN104477943A (en) | Method for preparing potassium sulfate | |
| CN1948236B (en) | Method of producing potassium ammonium sulfate compound fertilizer using potassium containing rock | |
| CN103539165A (en) | Method for producing potassium sulfate by utilizing insoluble rocks containing potassium | |
| CN103641748B (en) | A kind of recycle by-product hydrochloric acid prepares the method for methylsulphonic acid | |
| CN101439867A (en) | Method for extracting potassium carbonate from cabo and refining carbon | |
| CN104326990A (en) | Method for fluoridating and synthesizing 5-flucytosine by cytosine | |
| CN107265486B (en) | The method for preparing lithium carbonate using pelite containing lithium | |
| CN110078097A (en) | A kind of technique of instant solution process for preparing potassium nitrate by double decomposition | |
| CN110002474A (en) | Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product | |
| CN109231168B (en) | Method and device for reducing sulfuric acid content in hydrochloric acid and acetic acid by-products in chloroacetic acid production | |
| CN100509786C (en) | Comprehensive process for tail gas in glyphosate production | |
| CN113044857B (en) | Production process for preparing high-purity sodium cyanide or potassium cyanide with high yield | |
| CN105417556A (en) | Preparation method of ammonium bifluoride | |
| CN102731356A (en) | Thiourea cleaning production method | |
| CN102020293B (en) | Method for recovering reagent grade sodium nitrate from waste liquid generated in citric acid bismuth production | |
| CN109180416A (en) | The synthetic method of naphthalene system fluoro-containing intermediate 1- fluoronaphthalene | |
| CN101591255B (en) | Clean production process of iminodiacetic acid | |
| CN107721879A (en) | A kind of liquid caustic soda methyl alcohol mixed liquor is used for the method for the free ethanamidine of ethenylamidine hydrochloride | |
| CN113860331A (en) | Method for synthesizing high-activity potassium fluoride and co-producing sodium fluoride by using waste liquid as raw material | |
| CN107417307A (en) | A kind of preparation technology of water-soluble drip irrigation potassium sulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190712 |
|
| RJ01 | Rejection of invention patent application after publication |