CN1030445C - Process for decomposition of aqueous ammonium chloride solution and process for production of sodium carbonate - Google Patents
Process for decomposition of aqueous ammonium chloride solution and process for production of sodium carbonate Download PDFInfo
- Publication number
- CN1030445C CN1030445C CN 91110654 CN91110654A CN1030445C CN 1030445 C CN1030445 C CN 1030445C CN 91110654 CN91110654 CN 91110654 CN 91110654 A CN91110654 A CN 91110654A CN 1030445 C CN1030445 C CN 1030445C
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- Prior art keywords
- lime
- milk
- fraction
- ammonium chloride
- decomposition
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/10—Separation of ammonia from ammonia liquors, e.g. gas liquors
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/18—Preparation by the ammonia-soda process
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Dairy Products (AREA)
- Gas Separation By Absorption (AREA)
Abstract
Method for the decomposition of an aqueous ammonium chloride solution (13)by means of a milk of lime (19) containing dicalcium silicate, obtained fromlimestone containing silicon, wherein the solution (13) is treatedsuccessively in a first step (16), with a quantity of milk of lime (20)which is deficient with respect to the stoechiometric quantity required todecompose all the ammonium chloride and, in a second step (17), with theremainder (21) of the milk of lime. Use of the method in the treatment ofthe aqueous ammonium chloride solution (9) produced in the soda productionmethod with ammonia.
Description
The present invention relates to the decomposition method that a kind of purpose is to produce the aqueous ammonium chloride solution of ammonia.
Ammonia one alkaline process (also claiming solvay process) is to produce the most widely used a kind of commercial run of yellow soda ash (TE PANGHOU, the manufacturing of soda, the dedicated reference document of attached ammonia process, 1969, Hafner publishing company now; Zoran RANT, Die Erzougung Von Soda nach den Solvay-verfahren(The production of sodium carbonate by the Solvay proeess), 1968, Ferdinand Enke Verlag, Stuttgart).In this currently known methods, ammonia is dissolved in the aqueous solution of sodium-chlor, is handled with carbonated gas behind the generation ammoniacal brine, so that sodium bicarbonate crystallization thus.The sodium bicarbonate aqueous suspension that produces is filtered, in order that mixture is divided into solid carbonic acid chlorine sodium filter cake and mother liquor.Mother liquid obtained ammonia derivative, especially ammonium hydroxide and the ammonium chloride of containing.In order to obtain ammonia, it must be handled to decompose these derivatives subsequently, the ammonia that obtains is recycled to technological process.The decomposition of mother liquor ammonium chloride adopts milk of lime process normally effective.Milk of lime is made by unslaked lime, and unslaked lime to be Wingdale calcine in the limestone kiln that the back produces.The lime that the calcined limestone method is obtained is generally various impurity and stains, and these impurity are mainly derived from Wingdale, is used for the coke in limestone kiln and the refractory liner of kiln.Silicon-dioxide is the undesirable impurity of a kind of Wingdale.Really at least wherein some have been found, with Calucium Silicate powder CaOSiO
2, 2CaOSiO
2And 3CaOSiO
2Form is in combined with lime.
Because the Calucium Silicate powder that contains in the excessive hydrogen calcium oxide solution is reactive for the ammonium chloride right and wrong, so they will cause the decline of milk of lime utilising efficiency, thereby has also reduced the utilising efficiency of Wingdale.
The present invention overcomes this shortcoming by a kind of method is provided, and this method is that decomposing ammonium chloride improves the milk of lime utilising efficiency that contains Calucium Silicate powder.
Therefore, the present invention is relevant a kind of by means of containing silicic acid dicalcium (2CaOSiO
2) the milk of lime method of decomposing the ammonium chlorate aqueous solution; According to the present invention, described solution is handled continuously, and the milk of lime quantity not sufficient of using in the first step to be decomposing the necessary stoichiometry of whole ammonium chlorides, and uses remaining milk of lime in second step.
According to the inventive method, the source of aqueous ammonium chloride solution is not strict, normally above-mentioned ammonia process sodium bicarbonate crystalline mother liquor.
Obtain milk of lime by water hydration unslaked lime, unslaked lime is produced by the silica containing Wingdale of calcining, and general silicon-dioxide is greater than 1%(by weight), for example between 2-8%, silicon-dioxide is with combined Calucium Silicate powder CaOSiO
2, 2CaOSiO
2, 3CaOSiO
2Form exists.
According to the present invention, the processing of aqueous ammonium chloride solution is carried out in two steps continuously with milk of lime.The first step, milk of lime consumption are not enough to whole ammonium chlorides and decompose required accurate amount.Though the inventor does not wish to accept the constraint that opinion is explained, however they think in the time-continuing process of this method the first step, at acidic medium mesosilicic acid dicalcium by reaction
Decompose, the lime that discharges reacts with ammonium chloride immediately, by reaction
In second step, adding remaining milk of lime is that the still undecomposed ammonium chloride of the first step decomposes essential amount.
In the method for the invention, it is enough high that the deficiency of the first step milk of lime is wanted, so that obtain the enough acidity of reaction medium, Dicalcium Phosphate (Feed Grade) decomposed.For example, in the first step of method, spendable milk of lime amount is for decomposing the 30-70% of the required accurate weight of whole ammonium chlorides.Measure the pH of reaction medium, suitable this method of control of energy respectively goes on foot the respective amount of used milk of lime.
In a useful embodiment of the inventive method, milk of lime is divided into two kinds of big or small fractions, a coarse grain fraction, and a particulate fraction, the coarse grain fraction is used for the first step, and the particulate fraction was used for for second step.Improve milk of lime utilising efficiency even more remarkable by this embodiment of the invention.Determine to observe if all other conditions are identical, the Dicalcium Phosphate (Feed Grade) strong tendency in the milk of lime accumulates in the coarse grain fraction.In this embodiment of the inventive method, coarse fraction divides corresponding to mostly be most 125 μ m(such as 20-44 μ m by mesh size) fraction kept here of sieve, and fine fraction divides corresponding to the fraction by described sieve, and it is favourable controlling its separation in such a way by size.
The inventive method is applicable to decomposes contained ammonium chloride in the residual mother liquor, and described mother liquor is from the crystallization of above-mentioned ammonia process sodium bicarbonate.
Therefore, the production method of the also relevant a kind of yellow soda ash of the present invention, when using this method, the carbonated gas processing of ammoniacal brine, so that generate the aq suspension of sodium bicarbonate, treated aq suspension is divided into the solid sodium bicarbonate that is contained in wherein and contains the mother liquor of ammonium chloride, in order to generate yellow soda ash, sodium bicarbonate will pass through calcining, and mother liquor is handled so that decomposing ammonium chloride with milk of lime; According to present method, use the milk of lime that contains the silicic acid dicalcium, mother liquor divides two consecutive steps (as mentioned above) to be handled with milk of lime.
According to following explanation to the single numeral of accompanying drawing, feature of the present invention and details are more obvious, show that the synoptic diagram of the inventive method specific embodiment is suitable for ammonia process production yellow soda ash.
Umerical device in the synoptic diagram comprises ammonia absorption chamber 1, and then is carbonization chamber 2.Absorption chamber 1 is the post that adds the concentrated sodium chloride aqueous solution 3 and ammonia 4.Ammoniacal brine 5 is flowed out by chamber 1, enters carbonization chamber 2.Wherein, ammoniacal brine and carbonated gas 6 upstream recycle back.In chamber 2, ammoniacal brine is gradually by the hydrogen-carbonate salinization, and sodium bicarbonate aq suspension 7 is discharged thus, and aqueous sodium bicarbonate suspension input filter 8 is so that separate its contained solid sodium bicarbonate and mother liquor 9.Sodium bicarbonate 26 on the de-entrainment filter is transported to calcining kiln (not marking), obtains yellow soda ash after the thermolysis there.
Mother liquor 9 contains ammonium hydroxide and ammonium chloride, and recovery is rational.For reaching this purpose, mother liquor is delivered to distillation column 10, at the bottom of post, add vapour stream 11.In distillation column 10, the ammonium hydroxide decomposition obtains ammonia 12(at capital) and aqueous ammonium chloride solution 13.
In order to decompose wherein contained ammonium chloride, the aqueous solution 13 usefulness milk of limes 19 are handled.Used milk of lime 19 obtains by hydration unslaked lime, and unslaked lime derives from and adds the limestone kiln (not marking) contain silicon-dioxide [for example silicon-dioxide is 4%(weight meter)] Wingdale.Therefore, milk of lime 19 contains reactive lime and to the reactive lime of ammonium chloride right and wrong, the non-reacted lime of existence is its part, with Dicalcium Phosphate (Feed Grade) (2CaOSiO at least
2) the form existence.
According to the present invention, milk of lime feeds wet cyclone 15, and the milk of lime classification becomes coarse fraction and divides 20 and particulate fraction 21 there.The effect of gradation is to make Dicalcium Phosphate (Feed Grade) to be distributed between the big or small fraction 20 and 21 that does not wait.Most Dicalcium Phosphate (Feed Grade) concentrates on coarse grain fraction 20.This result is conspicuous according to following table, lists the amount of calcium and silicon in all cases in table by the big or small fraction of its clear regulation, and described big or small fraction obtains by the milk of lime gradation.
Size fraction calcium weight (g) silicon weight (g) silicon/calcium weight ratio
＞125μm????40.17????8.99????0.22
125-44μm????48.01????2.94????0.06
44-20μm????49.55????1.72????0.03
＜20μm????49.51????1.61????0.03
The downstream of distillation column 10, device comprise two reaction chambers 16 and 17.Reaction chamber 16 adds the coarse grain fraction 20 of the aqueous ammonium chloride solution 13 and the milk of lime that derive from post 10.The control all situations down solution 13 and the feed rate of milk of lime 20, adopt in such a way, promptly just decompose all with regard to the necessary amount of ammonium chloride of solution 13 feedings, the lime deficiency exists in chamber 16.Therefore, the reaction medium in the reaction chamber 16 has acidic character, and this helps the decomposition of Dicalcium Phosphate (Feed Grade), and the result is released reactive lime.Therefore, the ammonium chloride of solution 13 decomposes pro rata by existing amount of lime in chamber 16.Ammoniated gas 22 and contain in chamber 16 still the aqueous solution 23 of undecomposed ammonium chloride and discharge by chamber 16.The aqueous solution 23 is sent into reaction chamber 17 with 21 1 of milk of lime particulate fractions.
In chamber 17, the ammonium chloride of solution 23 is decomposed by the reactive lime of milk of lime 21.The aqueous solution 25 of ammoniated gas 24 and no ammonium chloride is discharged by chamber 17.The aqueous solution 25 and the air-flow 22 that is emitted by chamber 16 and 17 and 24 flow in the distillation columns 10.Post 10 top expellant gas 12 are circulated in the ammonia absorption chamber 1.
Claims (9)
1, the method for decomposition of aqueous ammonium chloride solution (13), wherein ammonium chloride and milk of lime reaction, it is characterized in that using and derive from the milk of lime that contains the silicic acid dicalcium (19) that contains greater than 1% (weight) silicon-dioxide and decomposition of limestone gained, processed continuously with described solution, is insufficient in the milk of lime amount of using in the first step (16) with regard to decomposing the necessary stoichiometry of whole ammonium chlorides, uses remaining milk of lime (21) in two steps (17).
2, by the method for claim 1, it is characterized in that used milk of lime derive from contain 2% and 8%(weight meter) between the decomposition of limestone of silicon-dioxide.
3, press the method for claim 1 or 2, it is characterized in that milk of lime (19) becomes two kinds of big or small fractions through gradation (15), it comprises coarse grain fraction (20) and particulate fraction (21), coarse grain fraction (20) be used for the first step (16) and particulate fraction (21) be used for second the step (17).
4, by the method for claim 3, the method that it is characterized in that controlling big or small gradation (15) is a coarse grain fraction (20) corresponding to the fraction of being kept here by the sieve of 125 μ m mesh sizes at the most, and particulate fraction (21) is corresponding to the fraction by this number sieve.
5, by the method for claim 4, the method that it is characterized in that controlling big or small gradation (15) be coarse grain fraction (20) corresponding to the fraction of being kept here by the sieve of mesh size between 20 and 44 μ m, and particulate fraction (21) is corresponding to the fraction by described sieve.
6,, it is characterized in that big or small gradation finishes in cyclone separator (15) by the method for claim 3.
7, by the method for claim 1, the amount that it is characterized in that the used milk of lime of the first step (16) (20) decompose all ammonium chlorides institute palpus milk of lime accurate weight 30% and 70% between.
8, by the method for claim 1, the measurement that it is characterized in that finishing reaction medium pH is to be applied to the amount that the first step (16) and second goes on foot (17) milk of lime mutually in order to control.
9, come free carbon dioxide containing gas to handle by the aqueous ammonium chloride solution that the process of claim 1 wherein and contain the mother liquor that ammoniated brine gained sodium bicarbonate aqeous suspension is removed the sodium bicarbonate post precipitation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE9000955 | 1990-10-10 | ||
| BE9000955A BE1004600A3 (en) | 1990-10-10 | 1990-10-10 | Aqueous ammonium chloride solution decomposition method and sodiumcarbonate production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1061760A CN1061760A (en) | 1992-06-10 |
| CN1030445C true CN1030445C (en) | 1995-12-06 |
Family
ID=3884962
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91110654 Expired - Fee Related CN1030445C (en) | 1990-10-10 | 1991-10-10 | Process for decomposition of aqueous ammonium chloride solution and process for production of sodium carbonate |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN1030445C (en) |
| BE (1) | BE1004600A3 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351216A (en) * | 2011-07-12 | 2012-02-15 | 湖南恒光科技股份有限公司 | Preparation process for soda ash capable of combined production of white carbon black |
| EP3006400B1 (en) * | 2014-10-09 | 2017-12-13 | Solvay SA | Process for producing ammonia |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE561500A (en) * | ||||
| US4294812A (en) * | 1978-05-25 | 1981-10-13 | General Electric Company | Recovery of ammonia from aqueous streams |
| JPS58172229A (en) * | 1982-04-02 | 1983-10-11 | Asahi Glass Co Ltd | Method for distilling ammonium chloride |
-
1990
- 1990-10-10 BE BE9000955A patent/BE1004600A3/en not_active IP Right Cessation
-
1991
- 1991-10-10 CN CN 91110654 patent/CN1030445C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1061760A (en) | 1992-06-10 |
| BE1004600A3 (en) | 1992-12-22 |
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