CN107792866B - A kind of method of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride - Google Patents
A kind of method of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride Download PDFInfo
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- CN107792866B CN107792866B CN201711195495.8A CN201711195495A CN107792866B CN 107792866 B CN107792866 B CN 107792866B CN 201711195495 A CN201711195495 A CN 201711195495A CN 107792866 B CN107792866 B CN 107792866B
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride, it is using alcohol-water mixed solution as solvent, a certain proportion of potassium alum is added to be dissolved with potassium chloride, potassium sulfate crystallization and potassium sulfate crystalline mother solution are obtained after metathesis reaction, potassium sulfate crystallization is washed, it is dry be finished product sulfuric acid potassium, potassium sulfate crystalline mother solution through evaporating, concentrating and crystallizing, separation of solid and liquid, wash, be dried to obtain finished product aluminium chloride.The present invention using potassium sulfate and aluminium chloride in ethanol different solubility the characteristics of, directly utilize the crystallization of potassium alum preparing potassium sulfate and aluminum chloride crystals, the problem of reaction condition is difficult to control when being produced which overcome tradition using water as solvent, potassium sulfate difficulty separates precipitation, and potassium aluminium high income, product purity are high, solvent easily recycles, low energy consumption, investing small, whole closing three-waste free discharge, the aluminium salt of directly production high added value, good in economic efficiency, device easily amplifies suitable for industrialization development.
Description
Technical field
The invention belongs to potassium sulfates and aluminium chloride production technical field, and in particular to a kind of potassium alum mixed solvent double decomposition
The method for producing potassium sulfate and aluminium chloride.
Background technique
Potassium is the highest cation of plant in-vivo content, to plant as one of needed for plant three big nutrients
Activation, photosynthesis, the adjusting of osmotic pressure, the synthesis of nutriment and operating of interior a variety of enzymes etc. play irreplaceable
Effect.But the universal potassium deficiency of China's major part soil, and long-term Potassium Fertilizer Application is insufficient, and the happiness potassium type farming sensitive to chloride ion
The growth of object can only apply chlorideless potassic fertilizer.Potassium sulfate contains 50% potassium oxide and 18% sulphur, as a kind of good chlorideless potassic fertilizer
Demand increases year by year.And China's potassium sulfate yield is unable to meet demand, needs a large amount of potassium sulfate of import every year.
The existing technique using potassium alum preparing potassium sulfate is mainly alum pyrolysismethod, normal pressure double decomposition.Alum pyrolysis
Method production potassium sulfate mainly has the workshop sections such as high-temperature roasting, water extraction, separation of solid and liquid, evaporating, concentrating and crystallizing, at 1000 DEG C or so
2h is roasted under high temperature and needs to consume a large amount of energy, and aluminum sulfate decomposites the SO come2、SO3Recovery difficult is high, to equipment requirement
Height easily causes environmental pollution, and a large amount of water need to be evaporated in evaporating, concentrating and crystallizing workshop section, and energy consumption is high.And normal pressure aqueous systems double decomposition
Since each ingredient such as potassium alum, potassium sulfate, aluminium chloride, potassium chloride is soluble easily in water in reaction system, opereating specification is very narrow, sulfuric acid
Potassium is not easy to be precipitated, and needing the amount of strict temperature control and reactant just can make product potassium sulfate few in system with crystalline state
Amount is precipitated, and product purity is not high, needs secondary purification that could obtain qualified potassium product, and equipment investment is big and production cost
It is high.
Summary of the invention
It cannot simply, efficiently be asked using the technology that potassium alum is converted into potassium sulfate and aluminium chloride to solve the prior art
Topic, the present invention provides a kind of methods of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride, utilize potassium sulfate
With the feature of aluminium chloride different solubility in ethanol solution so that reaction generate potassium sulfate directly in the form of solid crystal
It is precipitated, and aluminium chloride is dissolved in ethanol solution, mild condition short with process flow, evaporated water are few, solvent easily returns
It receives, product purity is high, directly prepare the aluminum chloride crystals of high added value, do not generate the three wastes, production equipment simply, low energy consumption, effect
The good advantage of benefit, therefore it is more suitable for industrialized production.
To achieve the above object, the present invention is implemented by following technical solution:
A kind of method of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride comprising following steps:
1) potassium alum, potassium chloride are added in alcohol-water mixed solution by certain mass ratio, stirring keeps its mixing equal
Even, then potassium sulfate crystallization is precipitated in a period of time of reaction at a certain temperature, and aluminium chloride is then dissolved in ethanol solution；
2) it is separated by solid-liquid separation at a certain temperature, obtains potassium sulfate crystallization and potassium sulfate crystalline mother solution, potassium sulfate is crystallized and is passed through
Washing, dry acquisition potassium product；
3) potassium sulfate crystalline mother solution obtained by step 2 is fallen to a certain temperature into acquisition aluminium chloride after flash vessel evaporation and concentration
Crystallization is separated by solid-liquid separation, obtains aluminum chloride crystals and aluminum chloride crystals mother liquor, aluminum chloride crystals are washed, dry to obtain chlorination
Aluminium product；
4) condensate liquid after being concentrated by evaporation potassium sulfate crystalline mother solution is used as with aluminum chloride crystals mother liquor back to step 1)
Mixed solution.
The mass ratio of potassium alum and potassium chloride is 1-3:1 in step 1).
The content of ethyl alcohol is 5-95wt% in alcohol-water mixed solution in step 1).
Reaction temperature is 50-90 DEG C in step 1), reaction time 30-90min.
The temperature being separated by solid-liquid separation in step 2 not less than 10 DEG C of metathesis reaction temperature to be advisable.
The temperature control of aluminum chloride crystals is at 30-80 DEG C in step 3), crystallization time 10-60min.
The condensate circulation after washing water and evaporation and concentration after aluminum chloride crystals mother liquor, wash crystallization is used as step 1)
Mixed solution.
The present invention compared with the method for existing potassium alum preparing potassium sulfate, the advantage is that:
(1) present invention potassium alum is directly dissolved in alcohol-water mixed solution, make its with ionic condition in the solution into
The crystallization of row potassium sulfate avoids the process that high-temperature roasting potassium alum is dehydrated it, greatly reduces energy consumption.
(2) present invention using potassium sulfate solubility in ethanol solution is small and aluminium chloride solubility in ethanol solution is big
Characteristic enables the potassium sulfate generated to be directly precipitated in large temperature range with solid crystalline state, and aluminium chloride is still dissolved in
In ethanol solution, so that potassium product single yield is higher, and can make the potassium product obtained purer, do not need
By secondary purification step, only high-purity sulfuric acid potassium can be obtained through being separated by solid-liquid separation, and ethyl alcohol is easy to evaporate recycling,
Be conducive to promote the crystallization of aluminium chloride to be precipitated.
(3) aluminium in the present invention is precipitated in the form of aluminum chloride crystals, is avoided high-temperature roasting and is decomposed aluminum sulfate and SO2、
SO3The process of absorption, and directly generated the high aluminium salt of added value rather than aluminium oxide, energy consumption is reduced, technique stream is shortened
Journey improves economic benefit, more environment-friendly and safer.
(4) relative to the evaporating, concentrating and crystallizing of other methods, the present invention made in a manner of adjusting temperature aluminum chloride crystals from
It is precipitated in ethanol solution, ethanol solution is recycled, and thus greatly reduces evaporated quantity of water, effectively reduces the energy consumption.
(5) present invention uses circulate operation, recycles each element in whole flow process, raw material availability height, potassium yield
It is high.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
25g potassium alum, 15g potassium chloride and 100g mixed solvent (ethanol content 90wt%) are added to sealing reactor
In, 50 DEG C are slowly heated to, mixing speed 200r/min makes to be uniformly mixed, and reacts 60min at such a temperature, then solid
Liquid separation, obtains 115g potassium sulfate crystalline mother solution and solid 1, solid 1 is washed, it is dry after obtain the crystallization of 20g potassium sulfate；By sulphur
Sour potassium crystalline mother solution adjusts temperature to 40 DEG C, low whipping speed is tied in the state of being 200r/min after flash vessel evaporation and concentration
After brilliant 40min, be separated by solid-liquid separation, obtain 100g aluminum chloride crystals mother liquor and solid 2, solid 2 is washed, it is dry after obtain 14g chlorine
Change crystalline aluminophosphate；Condensate liquid, the washing water after wash crystallization and aluminum chloride crystals mother liquor after potassium sulfate crystalline mother solution evaporation and concentration
The dissolution for being used for salt is returned after being evaporated to 100g.
Gained potassium sulfate contains potassium oxide 50.3%, chloride ion 1.4%, meets agricultural potassium sulfate primary standard, gained aluminium chloride
Purity meets industrial goods requirement for 93%.
Embodiment 2
35g potassium alum, 20g potassium chloride and 100g mixed solvent (ethanol content 80wt%) are added to sealing reactor
In, 60 DEG C are slowly heated to, mixing speed 200r/min makes to be uniformly mixed, and reacts 90min at such a temperature, then solid
Liquid separation, obtains 125g potassium sulfate crystalline mother solution and solid 1, solid 1 is washed, it is dry after obtain the crystallization of 25g potassium sulfate；By sulphur
Sour potassium crystalline mother solution adjusts temperature to 50 DEG C, low whipping speed is tied in the state of being 200r/min after flash vessel evaporation and concentration
After brilliant 40min, be separated by solid-liquid separation, obtain 110g aluminum chloride crystals mother liquor and solid 2, solid 2 is washed, it is dry after obtain 18g chlorine
Change crystalline aluminophosphate；Condensate liquid, the washing water after wash crystallization and aluminum chloride crystals mother liquor after potassium sulfate crystalline mother solution evaporation and concentration
The dissolution for being used for salt is returned after being evaporated to 100g.
Gained potassium sulfate contains potassium oxide 50.2%, chloride ion 1.4%, meets agricultural potassium sulfate primary standard, gained aluminium chloride
Purity meets industrial goods requirement for 94%.
Embodiment 3
40g potassium alum, 20g potassium chloride and 100g mixed solvent (ethanol content 70wt%) are added to sealing reactor
In, 70 DEG C are slowly heated to, mixing speed 200r/min makes to be uniformly mixed, and reacts 60min at such a temperature, then solid
Liquid separation, obtains 123g potassium sulfate crystalline mother solution and solid 1, solid 1 is washed, it is dry after obtain the crystallization of 22g potassium sulfate；By sulphur
Sour potassium crystalline mother solution adjusts temperature to 55 DEG C, low whipping speed is tied in the state of being 200r/min after flash vessel evaporation and concentration
After brilliant 40min, be separated by solid-liquid separation, obtain 102g aluminum chloride crystals mother liquor and solid 2, solid 2 is washed, it is dry after obtain 23g chlorine
Change crystalline aluminophosphate；Condensate liquid, the washing water after wash crystallization and aluminum chloride crystals mother liquor after potassium sulfate crystalline mother solution evaporation and concentration
The dissolution for being used for salt is returned after being evaporated to 100g.
Gained potassium sulfate contains potassium oxide 50.3%, chloride ion 1.2%, meets agricultural potassium sulfate primary standard, gained aluminium chloride
Purity meets industrial goods requirement for 93%.
Embodiment 4
30g potassium alum, 10g potassium chloride and 100g mixed solvent (ethanol content 85wt%) are added to sealing reactor
In, 70 DEG C are slowly heated to, mixing speed 200r/min makes to be uniformly mixed, and reacts 30min at such a temperature, then solid
Liquid separation, obtains 128g potassium sulfate crystalline mother solution and solid 1, solid 1 is washed, it is dry after obtain the crystallization of 15g potassium sulfate；By sulphur
Sour potassium crystalline mother solution adjusts temperature to 60 DEG C, low whipping speed is tied in the state of being 200r/min after flash vessel evaporation and concentration
After brilliant 40min, be separated by solid-liquid separation, obtain 107g aluminum chloride crystals mother liquor and solid 2, solid 2 is washed, it is dry after obtain 20g chlorine
Change crystalline aluminophosphate；Condensate liquid, the washing water after wash crystallization and aluminum chloride crystals mother liquor after potassium sulfate crystalline mother solution evaporation and concentration
The dissolution for being used for salt is returned after being evaporated to 100g.
Gained potassium sulfate contains potassium oxide 50.5%, chloride ion 1.4%, meets agricultural potassium sulfate primary standard, gained aluminium chloride
Purity meets industrial goods requirement for 95%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of method of potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride, it is characterised in that: including walking as follows
It is rapid:
1) potassium alum, potassium chloride are added in alcohol-water mixed solution by certain mass ratio, stirring is uniformly mixed it, so
Potassium sulfate crystallization is precipitated in a period of time of reaction at a certain temperature afterwards；
2) it is separated by solid-liquid separation at a certain temperature, obtains potassium sulfate crystallization and potassium sulfate crystalline mother solution, potassium sulfate crystallization is washed, dry
Dry acquisition potassium product；
3) potassium sulfate crystalline mother solution obtained by step 2 is fallen to a certain temperature after flash vessel evaporation and concentration and obtains aluminium chloride knot
Crystalline substance is separated by solid-liquid separation, obtains aluminum chloride crystals and aluminum chloride crystals mother liquor, aluminum chloride crystals are washed, dry to obtain aluminium chloride
Product；
The content of ethyl alcohol is 70-90wt% in alcohol-water mixed solution in step 1)；
The temperature control of aluminum chloride crystals is at 30-80 DEG C in step 3), crystallization time 10-60min.
2. the method for potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride according to claim 1, feature
Be: the mass ratio of potassium alum and potassium chloride is 1-3:1 in step 1).
3. the method for potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride according to claim 1, feature
Be: reaction temperature is 50-90 DEG C in step 1), reaction time 30-90min.
4. the method for potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride according to claim 1, feature
Be: the temperature being separated by solid-liquid separation in step 2 not less than 10 DEG C of metathesis reaction temperature to be advisable.
5. the method for potassium alum mixed solvent double decomposition production potassium sulfate and aluminium chloride according to claim 1, feature
Be: condensate liquid, the washing water after wash crystallization and aluminum chloride crystals mother liquor after potassium sulfate crystalline mother solution is concentrated by evaporation follow
Ring is used as the mixed solution of step 1).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167377A (en) * | 2010-11-30 | 2011-08-31 | 汪晋强 | Method for preparing aluminum chloride coproduced with potassium chloride and iron chloride by using vanadium slurry |
| CN104261433A (en) * | 2014-09-24 | 2015-01-07 | 湘潭市天志科技有限公司 | Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste |
| CN104743583A (en) * | 2015-04-24 | 2015-07-01 | 傅培鑫 | Method for producing potassium sulphate and aluminium chloride by utilizing potassium alum |
| CN106892442A (en) * | 2017-04-01 | 2017-06-27 | 福州大学 | A kind of method of potassium alum pressurization double decomposition production potassium sulfate and aluminium chloride |
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- 2017-11-24 CN CN201711195495.8A patent/CN107792866B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167377A (en) * | 2010-11-30 | 2011-08-31 | 汪晋强 | Method for preparing aluminum chloride coproduced with potassium chloride and iron chloride by using vanadium slurry |
| CN104261433A (en) * | 2014-09-24 | 2015-01-07 | 湘潭市天志科技有限公司 | Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste |
| CN104743583A (en) * | 2015-04-24 | 2015-07-01 | 傅培鑫 | Method for producing potassium sulphate and aluminium chloride by utilizing potassium alum |
| CN106892442A (en) * | 2017-04-01 | 2017-06-27 | 福州大学 | A kind of method of potassium alum pressurization double decomposition production potassium sulfate and aluminium chloride |
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Effective date of registration: 20230721 Address after: 336699 North of Qingyi Road, Chengxi Industrial Park, Fenyi County, Xinyu City, Jiangxi Province Patentee after: Xinyu Guoxing Lithium Industry Co.,Ltd. Address before: 350108 new campus of Fuzhou University, No. 2, Xue Yuan Road, University Town, Minhou street, Minhou, Fujian. Patentee before: FUZHOU University |