CN107934994A - A kind of preparation method of potassium sulfate - Google Patents
A kind of preparation method of potassium sulfate Download PDFInfo
- Publication number
- CN107934994A CN107934994A CN201810026494.9A CN201810026494A CN107934994A CN 107934994 A CN107934994 A CN 107934994A CN 201810026494 A CN201810026494 A CN 201810026494A CN 107934994 A CN107934994 A CN 107934994A
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- China
- Prior art keywords
- reaction
- ammonium sulfate
- potassium
- mother liquor
- sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/08—Preparation of sulfates by double decomposition with each other or with ammonium sulfate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Fertilizers (AREA)
Abstract
The present invention provides a kind of preparation method of potassium sulfate, meets that ammonium sulfate is produced in Process of Potassium Sulfate to temperature and reactivity needs with potassium chloride double decomposition using the reaction heat and chemical reactivity of the generation of the vigorous reaction of sulfuric acid and ammonia.The exothermic heat of reaction of liquefied ammonia and sulfuric acid is extremely violent, and central reaction temperature moment, substantial amounts of reaction heat, Q=174.72kJ/mol were released in reaction up to 1291 DEG C.Substantial amounts of reaction heat is released using liquefied ammonia and sulfuric acid reaction, to complete the required heat of whole potassium sulfate production process heating, any external heat source is not required in whole production process, due to being to be passed through liquid ammonia and sulfuric acid under agitation, the two reacts and releases reaction heat, the warm-up movement of each ion is improved in reaction zone, so that temperature of charge and reactivity are increased sharply, raw material sulphuric acid ammonium is set to dissolve rapidly, the metathesis reaction after dissolving with potassium chloride in reactive tank is rapidly completed.
Description
Technical field
The present invention relates to a kind of preparation method of potassium sulfate, belong to the preparing technical field of composite fertilizer's potassium sulfate.
Background technology
Potassium sulfate is a kind of important basic chemical raw materials, is the main production raw material of sulfenyl fertilizer in composite fertilizer.China's soil
84% potassium deficiency of ground, while China is the very deficient country of a potassium resource again, thus limit utilization and the hair of potash fertilizer
Exhibition.Cause the serious disproportion of crops soil Main Nutrients N P and K.The principal item of potash fertilizer have potassium chloride, potassium sulfate,
Potassium nitrate, since fear-chlorion crop cannot apply potassium chloride, potassium nitrate is expensive, and is explosive, using being restricted.And sulfuric acid
Potassium can also provide the potassium and sulphur of crop needs at the same time, be particularly appropriate for fear-chlorion crop, cheap.Therefore chlorideless potassic fertilizer is with potassium sulfate
Based on.
Since 2013, the demand sharp increase of China's agricultural fertilizer industry, especially composite fertilizer's industry to potassium sulfate, locates at present
State that supply falls short of demand.
A kind of preparation method of potassium sulfate and ammonium chloride disclosed in patent 201610720769X, it is relative to traditional sulphur
Sour potassium and potassium chloride double decomposition, has been realized in consecutive production, and has many advantages such as energy saving, small investment, efficiency height,
But it is not optimal, metathesis process production potassium sulfate process, raw material is reacted in reaction medium water, this process
It is middle to need to heat to promote the dissolving of ammonium sulfate, and need at least 30min to complete course of dissolution, under heating with potassium chloride
Reaction, needs time 15min with chlorination nak response.
The content of the invention
The deficiency for more than, the present invention provide a kind of preparation method of efficient, energy saving potassium sulfate.
The present invention is implemented by the following technical programs：A kind of preparation method of potassium sulfate, comprises the following steps：
（1）Mother liquor or clear water well prepared in advance are added in ammonium sulfate liquid pool by proportioning, while will pass through and crush,
Ammonium sulfate after screening, metering is sent in ammonium sulfate liquid pool；
（2）Sulfuric acid and liquefied ammonia through metering are added into ammonium sulfate liquid pool, sulfuric acid and liquefied ammonia occur acutely by stirring
Reaction, makes ammonium sulfate quickly dissolve；
（3）Dissolved ammonium sulfate and the potassium chloride after sieving, measuring are sent in reactive tank and carry out double decomposition
Reaction；
（4）The slurry overflow that metathesis reaction is produced, which enters in long brilliant groove, is further reacted and long brilliant；
（5）By step（4）Obtained mixing liquid overflow, which enters, carries out solid-liquid sedimentation separation in thickener, clear liquid flows into hot mother liquor
In groove, precipitation slurry is separated into major product centrifuge, obtains solid sulphuric acid potassium；
（6）Clear liquid in hot mother liquor groove is sent into the cooling bath equipped with circulation cold medium oil and is cooled down under agitation, mother liquor cooling
Crystallization separates out byproduct afterwards；And the Medium Oil after exchanging heat from mixed liquor since density is different, separate and be sent into cooling system
System carries out kind of refrigeration cycle use；Mother liquor and ammonium chloride mixt is crystallized out, be sent in thickener and carry out separation of solid and liquid, separated
Obtained clear liquid is overflowed in mother liquor holding tank and recycled for preparing ammonium sulfate, the mixing such as solid ammonium chloride of stiff
Thing, isolates the mixtures such as solid ammonium chloride, obtained separating liquid is equally entered into mother liquor holding tank into byproduct centrifuge
Recycled for preparing ammonium sulfate.
Step（3）In, when ammonium sulfate and potassium chloride complete metathesis reaction after, protected by adjusting the addition of ammonia
The pH value of solution is demonstrate,proved in the range of 6-8.
The present invention is to meet ammonium sulfate using the reaction heat and chemical reactivity of the generation of the vigorous reaction of sulfuric acid and ammonia
Being produced with potassium chloride double decomposition in Process of Potassium Sulfate needs temperature and reactivity.In ammonium sulfate course of dissolution, sulfuric acid is added
And liquefied ammonia is passed through, the exothermic heat of reaction of liquefied ammonia and sulfuric acid is extremely violent, and central reaction temperature moment, reaction was released big up to 1291 DEG C
The reaction heat of amount, Q=- 174.72kJ/mol.Substantial amounts of reaction heat is released using liquefied ammonia and sulfuric acid reaction, to complete whole sulfuric acid
The required heat of potassium production process heating, any external heat source is not required in whole production process, due to being to be passed through under agitation
Liquid ammonia and sulfuric acid, the two reacts and releases reaction heat, the warm-up movement of each ion is improved in reaction zone, so that reactant
Temperature and reactivity are increased sharply, and ammonium sulfate is dissolved rapidly, the metathesis reaction after dissolving in reactive tank with potassium chloride
It is rapidly completed.
The present invention takes full advantage of the reaction heat of the concentrated sulfuric acid and the generation of liquefied ammonia vigorous reaction and its activity of reaction product, makes
Reaction speed greatly improves, and whole reaction process provides thermal energy without exterior, saves energy and reaction time that heating needs,
Substantially reduce production cost.
Embodiment
A kind of preparation method of potassium sulfate, comprises the following steps：
（1）Mother liquor or clear water well prepared in advance are added in ammonium sulfate liquid pool by proportioning, while will pass through and crush,
Ammonium sulfate after screening, metering is sent in ammonium sulfate liquid pool；
（2）Sulfuric acid and liquefied ammonia through metering are added into ammonium sulfate liquid pool, sulfuric acid and liquefied ammonia occur acutely by stirring
Reaction, makes ammonium sulfate quickly dissolve；
（3）Dissolved ammonium sulfate and the potassium chloride after sieving, measuring are sent in reactive tank and carry out double decomposition
Reaction；After ammonium sulfate and potassium chloride complete metathesis reaction, ensure the pH value of solution by adjusting the addition of ammonia
In the range of 6-8；
（4）The slurry overflow that metathesis reaction is produced, which enters in long brilliant groove, is further reacted and long brilliant；
（5）By step（4）Obtained mixing liquid overflow, which enters, carries out solid-liquid sedimentation separation in thickener, clear liquid flows into hot mother liquor
In groove, precipitation slurry is separated into major product centrifuge, obtains solid sulphuric acid potassium；
（6）Clear liquid in hot mother liquor groove is sent into the cooling bath equipped with circulation cold medium oil and is cooled down under agitation, mother liquor cooling
Crystallization separates out byproduct afterwards；And the Medium Oil after exchanging heat from mixed liquor since density is different, separate and be sent into cooling system
System carries out kind of refrigeration cycle use；Mother liquor and ammonium chloride mixt is crystallized out, be sent in thickener and carry out separation of solid and liquid, separated
Obtained clear liquid is overflowed in mother liquor holding tank and recycled for preparing ammonium sulfate, the mixing such as solid ammonium chloride of stiff
Thing, isolates the mixtures such as solid ammonium chloride, obtained separating liquid is equally entered into mother liquor holding tank into byproduct centrifuge
Recycled for preparing ammonium sulfate.
Preparation of the reaction heat and its activity of reaction product produced for the concentrated sulfuric acid and liquefied ammonia vigorous reaction to potassium sulfate
The influence brought, makees analysis below explanation：
2NH3+H2SO4=（NH4）2SO4+ΔHmө=-174.72kJ/mol
34g 98g 132g
1kg mother liquors, which raise 1 degree, needs 3.15kj heats, and 3150j/kg DEG C of the specific heat capacity of mother liquor, producing 3.5 tons of ammonium sulfate can produce
Heat amount 4632727kj；Heat up 70 degree for 21 tons of mother liquors.
Producing 5 ton hour of potassium sulfate needs 3.5 tons of ammonium sulfate.Normal production and application mother liquor and ammonium sulfate combined amount about 12
Ton hour, heat up 70 DEG C of calorific requirement 2646000kj, need to put into 1.59 ton of 93% sulfuric acid, 0.51 ton of liquefied ammonia, can produce 2 tons of sulfuric acid
Ammonium salt solution and 2641406kj heats, put into 1.5 tons of solid ammonium sulfates, the adjustable liquefied ammonia of actual temperature control and sulfuric acid with
The proportional quantity control of solid ammonium sulfate.
Claims (2)
1. a kind of preparation method of potassium sulfate, it is characterised in that comprise the following steps：
（1）Mother liquor or clear water well prepared in advance are added in ammonium sulfate liquid pool by proportioning, while will pass through and crush,
Ammonium sulfate after screening, metering is sent in ammonium sulfate liquid pool；
（2）Sulfuric acid and liquefied ammonia through metering are added into ammonium sulfate liquid pool, sulfuric acid and liquefied ammonia occur acutely by stirring
Reaction, makes ammonium sulfate quickly dissolve；
（3）Dissolved ammonium sulfate and the potassium chloride after sieving, measuring are sent in reactive tank and carry out double decomposition
Reaction；
（4）The slurry overflow that metathesis reaction is produced, which enters in long brilliant groove, is further reacted and long brilliant；
（5）By step（4）Obtained mixing liquid overflow, which enters, carries out solid-liquid sedimentation separation in thickener, clear liquid flows into hot mother liquor
In groove, precipitation slurry is separated into major product centrifuge, obtains solid sulphuric acid potassium；
（6）Clear liquid in hot mother liquor groove is sent into the cooling bath equipped with circulation cold medium oil and is cooled down under agitation, mother liquor cooling
Crystallization separates out byproduct afterwards；And the Medium Oil after exchanging heat from mixed liquor since density is different, separate and be sent into cooling system
System carries out kind of refrigeration cycle use；Mother liquor and ammonium chloride mixt is crystallized out, be sent in thickener and carry out separation of solid and liquid, separated
Obtained clear liquid is overflowed in mother liquor holding tank and recycled for preparing ammonium sulfate, the mixing such as solid ammonium chloride of stiff
Thing, isolates the mixtures such as solid ammonium chloride, obtained separating liquid is equally entered into mother liquor holding tank into byproduct centrifuge
Recycled for preparing ammonium sulfate.
A kind of 2. preparation method of potassium sulfate as claimed in claim 1, it is characterised in that：Step（3）In, work as ammonium sulfate
After completing metathesis reaction with potassium chloride, ensure the pH value of solution in the range of 6-8 by adjusting the addition of ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810026494.9A CN107934994A (en) | 2018-01-11 | 2018-01-11 | A kind of preparation method of potassium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810026494.9A CN107934994A (en) | 2018-01-11 | 2018-01-11 | A kind of preparation method of potassium sulfate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100699A (en) * | 1993-09-23 | 1995-03-29 | 南京化学工业(集团)公司研究院 | Method for prodn. of potassium sulphate using ammonium sulphate and potassium chloride |
| CN106335910A (en) * | 2016-08-25 | 2017-01-18 | 辽宁津大肥业有限公司 | Potassium sulfate and ammonium chloride preparation method |
-
2018
- 2018-01-11 CN CN201810026494.9A patent/CN107934994A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100699A (en) * | 1993-09-23 | 1995-03-29 | 南京化学工业(集团)公司研究院 | Method for prodn. of potassium sulphate using ammonium sulphate and potassium chloride |
| CN106335910A (en) * | 2016-08-25 | 2017-01-18 | 辽宁津大肥业有限公司 | Potassium sulfate and ammonium chloride preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 王正银主编: "《肥料研制与加工》", 31 December 2015, 中国农业大学出版社 * |
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Application publication date: 20180420 |