CN104743583B - A kind of method that utilization potassium alum produces potassium sulfate and aluminum chloride - Google Patents
A kind of method that utilization potassium alum produces potassium sulfate and aluminum chloride Download PDFInfo
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- CN104743583B CN104743583B CN201510197669.9A CN201510197669A CN104743583B CN 104743583 B CN104743583 B CN 104743583B CN 201510197669 A CN201510197669 A CN 201510197669A CN 104743583 B CN104743583 B CN 104743583B
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- potassium sulfate
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Abstract
The present invention relates to a kind of method that utilization potassium alum produces potassium sulfate and aluminum chloride, the material that the method is selected is potassium alum and potassium chloride and the water as solvent, and the weight of potassium alum and potassium chloride ratio is for 1.5 2.5:1, production method includes potassium alum/potassium chloride complex decomposition reactive crystallization method preparing potassium sulfate stage and evaporating, concentrating and crystallizing produces the aluminum chloride stage, the preparing potassium sulfate stage can be 1 time or circulate several times, in the above-mentioned stage, metathesis reaction temperature >=60 DEG C, response time >=20 min, solid-liquid separation holding temperature >=50 DEG C, evaporating, concentrating and crystallizing temperature >=90 DEG C.The method, compared with the existing method using potassium alum production potassium sulfate and aluminum chloride, has technological process short（One step conversion）, solid-liquid separation is easy, energy consumption is low, the beneficial effect such as non-environmental-pollution, low production cost, easy industrializing implementation, utilization of materials height.
Description
Technical field
The invention belongs to potassium sulfate and aluminum chloride production technical field, more particularly, to one kind produce potassium sulfate using potassium alum
Method with aluminum chloride.
Background technology
Potassium alum is a kind of potassium aluminium sulfate double salt, and molecular formula is K2SO4·Al2(SO4)3·24H2O.
The method that existing utilization potassium alum produces potassium sulfate and aluminum chloride, has Alumen pyrolysismethod, Alumen ammonolysis process, Alumen hydrogen
Potassium oxide displacement method etc..
Alumen pyrolysismethod produces potassium sulfate and aluminium oxide, and master operation is dehydrated for Alumen（Generate dried Alumen, i.e. alumen exsiccatum）、
Thermal decomposition, desulfurization, hot water leaching, solid-liquid separation, evaporating, concentrating and crystallizing.Existing problems, one is high energy consumption.Alumen is dehydrated（300—
400 DEG C, dehydration fever 1455KJ/Kg）, thermal decomposition（500 600 DEG C, decomposition heat 620KJ/Kg）, aluminum sulfate decompose（760—800
DEG C, the hot 980KJ/Kg of desulfurization）.Two is environmental pollution.Desulphurization reaction produces SO3Pollution environment.Three is that technology difficulty is big.Alumen takes off
Water process occurs certainly to stick and expanded, and technological process length, difficulty are big.Four is that leaching liquid evaporation and concentration extracts potassium sulfate, evaporated water
Many, high energy consumption.
Alumen ammonolysis craft method produces potassium-nitrogen fertilizer and aluminium hydroxide, and master operation is ammonia（Liquefied ammonia, ammonia）Decompose Alumen（Jljl
The factors such as material proportioning, reaction temperature, Alumen granularity, ammonia concn are relevant）, generate aluminium hydroxide and potassium sulfate（Ammonium）Mother solution.Deposit
In problem, one is NH3Reclaim and environmental pollution.Two is gel aluminium hydroxide filtration difficulty, and high-temperature roasting energy consumption is big.Three is sulfur
Sour potassium（Ammonium）Mother solution amount is big, evaporation and concentration high energy consumption, and potassium-nitrogen fertilizer added value is low.
Alumen potassium hydroxide displacement method produces potassium sulfate and aluminium hydroxide, and master operation is put with alum solution for potassium hydroxide
Change reaction, generate aluminium hydroxide and potassium sulfate.Existing problems, one is the gel aluminum hydroxide shape generating, and solid-liquid separation is difficult.Two
It is that production cost is high.Three is that potassium sulfate mother liquid amount is big, evaporating, concentrating and crystallizing high energy consumption.
Content of the invention
For overcoming existing utilization potassium alum to produce the above-mentioned subject matter of the method presence of potassium sulfate and aluminum chloride, the present invention
Technical problem to be solved is：A kind of method that brand-new utilization potassium alum produces potassium sulfate and aluminum chloride is provided.
The technical solution adopted in the present invention is：A kind of method that utilization potassium alum produces potassium sulfate and aluminum chloride, it is special
Levying is：The material that the method is selected is potassium alum and potassium chloride, and the weight of potassium alum and potassium chloride ratio is for 1.5-2.5:1, its life
Product method was included as the next stage：
（1）, potassium alum/potassium chloride complex decomposition reactive crystallization method preparing potassium sulfate stage
This stage includes for the potassium alum of described ratio and potassium chloride being placed in heating for dissolving in appropriate water, potassium alum/chlorine
Change potassium metathesis reaction, solid-liquid separation obtains crystalline sulfuric acid potassium and the operation of the first crystalline mother solution, wherein metathesis reaction temperature
>=60 DEG C, response time >=20 min, solid-liquid separation holding temperature >=50 DEG C, the above-mentioned preparing potassium sulfate stage is 1 time or circulation
Several times；The first crystalline mother solution being obtained through 1 preparing potassium sulfate stage is directly entered and produces the aluminum chloride stage（Referred to as
Method 1）；For the circulation preparing potassium sulfate stage several times, the crystalline sulfuric acid obtaining each time potassium is collected, will be female for the first crystallization
Liquid returns above-mentioned preparing potassium sulfate system, and adds the material with starting stage same component and weight in system, repeat on
State potassium alum/potassium chloride metathesis reaction and potassium sulfate separation process, through potassium alum several times/potassium chloride metathesis reaction and sulfur
First crystalline mother solution of the enrichment aluminum chloride that sour potassium separation process obtains, enters back into and produces the aluminum chloride stage（Abbreviation method 2）；Produce
The crystalline sulfuric acid potassium going out washes with water, and drying obtains potassium sulfate finished product；
（2）, evaporating, concentrating and crystallizing produce the aluminum chloride stage
The first described crystalline mother solution is passed through to heat stirring, evaporating, concentrating and crystallizing, solid-liquid separation, obtains aluminum chloride and the
Two crystalline mother solutions, evaporating, concentrating and crystallizing temperature >=90 DEG C.
The preferred version of the present invention is：The weight of described potassium alum and potassium chloride is than for 2:1.Described metathesis reaction temperature
For 60-85 DEG C, the response time is 20-80min, and solid-liquid separation holding temperature is 50-70 DEG C, and evaporating, concentrating and crystallizing temperature is 90-
100℃.
The invention has the advantages that：The method that the method produces potassium sulfate and aluminum chloride with existing utilization potassium alum
Compare, there is technological process short（One step conversion）, solid-liquid separation is easy, energy consumption is low, non-environmental-pollution, low production cost, Yi Gong
The beneficial effects such as industry enforcement, utilization of materials height.
Below in conjunction with the accompanying drawings and specific embodiment the invention will be further described.
Brief description
Fig. 1 is present invention process schematic flow sheet.
Specific embodiment
Embodiment 1
The present embodiment adopts method 1, is directly entered system through the first crystalline mother solution that 1 preparing potassium sulfate stage is obtained
Take the aluminum chloride stage.
From material：100 grams of potassium alum, 50 grams of potassium chloride and the suitable quantity of water as solvent（Water of crystallization containing potassium alum, under
With）, the water yield can be completely dissolved selection with material, and the present embodiment water is 250 grams.100 grams of above-mentioned potassium alum, 50 grams of potassium chloride is reason
Stoichiometric, actual amount is the 100-110% of theoretical amount.Its preparation method was included as the next stage：
（1）, potassium alum/potassium chloride complex decomposition reactive crystallization method preparing potassium sulfate stage：
100 grams of potassium alums and 50 grams of potassium chloride are placed in heating for dissolving in 250 grams of water, are sufficiently stirred for, treat that material is completely molten
Xie Hou, by potassium alum/potassium chloride metathesis reaction, solid-liquid separation, obtains 70 grams about of potassium sulfate and the first crystalline mother solution
250ml about, the first crystalline mother solution being obtained is directly entered produces the aluminum chloride stage.Wherein, material heating for dissolving temperature with
Material can be made to be completely dissolved setting, usually 70-100 DEG C；Metathesis reaction temperature is 60-85 DEG C, and the response time is 20-
80min, metathesis reaction temperature is higher, then the response time is shorter, can select optimum process technology parameter by practical situation；Gu
Liquid separation holding temperature is 50-70 DEG C.The first separating obtained crystalline mother solution contains aluminum chloride, potassium alum, potassium chloride, incomplete
The potassium sulfate separating out and water.The crystalline sulfuric acid potassium of output washes with water, and drying obtains potassium sulfate finished product, and washing liquid is incorporated to
One crystalline mother solution returns preparing potassium sulfate system, heating for dissolving potassium alum and potassium chloride, recycles, improve further resource/
Energy utilization rate.
（2）, evaporating, concentrating and crystallizing produce aluminum chloride：
By the first crystalline mother solution by heat stirring, evaporating, concentrating and crystallizing, solid-liquid separation, obtain aluminum chloride and the second crystallization
Mother solution, evaporating, concentrating and crystallizing temperature is 90-100 DEG C.The second crystalline mother solution that solid-liquid separation obtains returns preparing potassium sulfate system,
Heating for dissolving potassium alum and potassium chloride, recycle.
Embodiment 2
The present embodiment adopts method 2, that is, circulate the preparing potassium sulfate stage several times.
（1）, potassium alum/potassium chloride complex decomposition reactive crystallization method preparing potassium sulfate stage：
From material：100 grams of potassium alum, 50 grams of potassium chloride and the suitable quantity of water as solvent（Water containing alum crystallisation, under
With）, the water yield can be completely dissolved selection with material, and the present embodiment water is 250 grams.100 grams of above-mentioned potassium alum, 50 grams of potassium chloride is reason
Stoichiometric, actual amount is the 100-110% of theoretical amount.Its preparation method was included as the next stage：
First 100 grams of potassium alums and 50 grams of potassium chloride are placed in heating for dissolving in 250 grams of water, are sufficiently stirred for, treat that material is complete
After CL, by potassium alum/potassium chloride metathesis reaction, solid-liquid separation, obtain 70 grams about of first part of crystalline sulfuric acid potassium and
First part of first crystalline mother solution 250ml about, first part of first crystalline mother solution is returned above-mentioned preparing potassium sulfate system, and in body
Add the material of same component and weight with the first stage in system（I.e. 100 grams of potassium alums and 50 grams of potassium chloride）, by the first hyposynchronization
Rapid and condition, i.e. heating for dissolving, are sufficiently stirred for, after material is completely dissolved, anti-by second potassium alum/potassium chloride double decomposition
Should, solid-liquid separation, obtain 70 grams about and second part of first crystalline mother solution 250ml about of second part of crystalline sulfuric acid potassium, by second
Part first crystalline mother solution returns above-mentioned preparing potassium sulfate system and carries out the third time preparing potassium sulfate stage, by that analogy, if repeating
Dry time.Through potassium alum several times/potassium chloride metathesis reaction and potassium sulfate separation process, obtain crystalline sulfuric acid potassium accumulation and richness
First crystalline mother solution of collection aluminum chloride, the first crystalline mother solution of this enrichment aluminum chloride enters subsequent produces the aluminum chloride stage.Tired
The crystalline sulfuric acid potassium of long-pending output washes with water, and drying obtains potassium sulfate finished product, and washing liquid is incorporated to the first crystalline mother solution return and produces
Potassium sulfate system, heating for dissolving potassium alum and potassium chloride, recycle, and improve resource/energy utilization rate further.
（2）, evaporating, concentrating and crystallizing produce aluminum chloride：
By the enrichment obtaining through potassium alum several times/potassium chloride metathesis reaction and potassium sulfate separation process aluminum chloride the
One crystalline mother solution, by heat stirring, evaporating, concentrating and crystallizing, solid-liquid separation, obtains aluminum chloride and the second crystalline mother solution, and evaporation is dense
Contracting crystallization temperature is 90-100 DEG C.The second crystalline mother solution that solid-liquid separation obtains returns preparing potassium sulfate system, heating for dissolving potassium
Alumen and potassium chloride, recycle.
In above-described embodiment, embodiment 2 can obtain the first crystalline mother solution of enrichment aluminum chloride compared with embodiment 1, carries further
Concentration of aluminum chloride in high first crystalline mother solution, simplification of flowsheet, improve production efficiency, reduces production cost.
The chemical equation of above-described embodiment is：（1）、 K2SO4· Al2(SO4)3·24H2O+6KCl+W1=4K2SO4
+ 2AlCl3+ W2.Wherein W1For the additional water yield, W2For system total Water, it is additional water yield W1With alum crystallisation water sum.（2）、
First crystalline mother solution-W3=AlCl3·6H2O+ second crystalline mother solution.Wherein W3For evaporated water.
Above-described embodiment is only the specific embodiment mode of the present invention, the technical data being directed to, and can set
Selected depending on concrete condition in fixed scope and mated.
Claims (9)
1. a kind of method that utilization potassium alum produces potassium sulfate and aluminum chloride, is characterized in that：The material that the method is selected is that potassium is bright
Vitriol and potassium chloride, the weight of potassium alum and potassium chloride is than for 1.5-2.5:1, its production method was included as the next stage：
（1）, potassium alum/potassium chloride complex decomposition reactive crystallization method preparing potassium sulfate stage
This stage includes for the potassium alum of described ratio and potassium chloride being placed in heating for dissolving in appropriate water, potassium alum/potassium chloride
Metathesis reaction, solid-liquid separation obtain crystalline sulfuric acid potassium and the operation of the first crystalline mother solution, wherein metathesis reaction temperature >=60
DEG C, response time >=20 min, solid-liquid separation holding temperature >=50 DEG C, the above-mentioned preparing potassium sulfate stage is 1 time or circulation is some
Secondary；The first crystalline mother solution being obtained through 1 preparing potassium sulfate stage is directly entered and produces the aluminum chloride stage；For circulation
In the preparing potassium sulfate stage several times, the crystalline sulfuric acid obtaining each time potassium is collected, the first crystalline mother solution is returned above-mentioned producing
Potassium sulfate system, and add the material with starting stage same component and weight in system, repeat above-mentioned potassium alum/potassium chloride
Metathesis reaction and potassium sulfate separation process, obtain through potassium alum several times/potassium chloride metathesis reaction and potassium sulfate separation process
First crystalline mother solution of the enrichment aluminum chloride arriving, enters back into and produces the aluminum chloride stage；The crystalline sulfuric acid potassium of output washes with water, warp
It is dried, obtain potassium sulfate finished product；
（2）, evaporating, concentrating and crystallizing produce the aluminum chloride stage
By the first described crystalline mother solution by heat stirring, evaporating, concentrating and crystallizing, solid-liquid separation, obtain aluminum chloride and the second knot
Brilliant mother solution, evaporating, concentrating and crystallizing temperature >=90 DEG C.
2. the method that utilization potassium alum according to claim 1 produces potassium sulfate and aluminum chloride, is characterized in that：Described potassium is bright
The weight of vitriol and potassium chloride is than for 2:1.
3. the method that utilization potassium alum according to claim 1 and 2 produces potassium sulfate and aluminum chloride, is characterized in that：Described
Metathesis reaction temperature is 60-85 DEG C, and the response time is 20-80min, and solid-liquid separation holding temperature is 50-70 DEG C, evaporation and concentration
Crystallization temperature is 90-100 DEG C.
4. the method that utilization potassium alum according to claim 1 and 2 produces potassium sulfate and aluminum chloride, is characterized in that：Described
Second crystalline mother solution returns above-mentioned preparing potassium sulfate system.
5. the method that utilization potassium alum according to claim 3 produces potassium sulfate and aluminum chloride, is characterized in that：Described second
Crystalline mother solution returns above-mentioned preparing potassium sulfate system.
6. the method that utilization potassium alum according to claim 1 and 2 produces potassium sulfate and aluminum chloride, is characterized in that：Described
Washing liquid after the crystalline sulfuric acid potassium of output washes with water is incorporated to the first crystalline mother solution return preparing potassium sulfate system.
7. the method that utilization potassium alum according to claim 3 produces potassium sulfate and aluminum chloride, is characterized in that：Described output
Crystalline sulfuric acid potassium wash with water after washing liquid be incorporated to first crystalline mother solution return preparing potassium sulfate system.
8. the method that utilization potassium alum according to claim 4 produces potassium sulfate and aluminum chloride, is characterized in that：Described output
Crystalline sulfuric acid potassium wash with water after washing liquid be incorporated to first crystalline mother solution return preparing potassium sulfate system.
9. the method that utilization potassium alum according to claim 5 produces potassium sulfate and aluminum chloride, is characterized in that：Described output
Crystalline sulfuric acid potassium wash with water after washing liquid be incorporated to first crystalline mother solution return preparing potassium sulfate system.
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| CN106430268B (en) * | 2016-10-08 | 2017-10-17 | 山西大学 | A kind of method that high-purity Aluminum Chloride Hexahydrate is extracted from mixed liquor |
| CN106395874B (en) * | 2016-10-08 | 2017-08-25 | 山西大学 | A kind of method that sodium chloride and Aluminum Chloride Hexahydrate are extracted from mixed liquor |
| CN106892442B (en) * | 2017-04-01 | 2018-07-20 | 福州大学 | A kind of method of potassium alum pressurization double decomposition production potassium sulfate and aluminium chloride |
| CN107792866B (en) * | 2017-11-24 | 2019-08-09 | 福州大学 | A kind of method of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride |
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| CN103466662B (en) * | 2013-09-23 | 2015-04-01 | 河北工业大学 | Method for preparing potassium sulfate with large grain diameter by utilizing reaction crystallization |
| CN103818935A (en) * | 2014-01-13 | 2014-05-28 | 赵凿元 | Method for separating potassium oxide from potassium-containing sodium aluminate solution |
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