CN109911919A - Potassium sulfate preparation system and method - Google Patents
Potassium sulfate preparation system and method Download PDFInfo
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- CN109911919A CN109911919A CN201711329164.9A CN201711329164A CN109911919A CN 109911919 A CN109911919 A CN 109911919A CN 201711329164 A CN201711329164 A CN 201711329164A CN 109911919 A CN109911919 A CN 109911919A
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Abstract
A kind of preparation method of potassium sulfate, include the following steps: S1: ammonium sulfate is added in salt dissolving groove to the solution for being configured to ammonium sulfate concentrations and reaching saturation, then the solution in salt dissolving groove is introduced into crystallizer, and solid potassium chloride is added in crystallizer and is reacted with solution and forms crystallization；S2: the solution after reacting in S1 step and crystal are subjected to Gravity Separation, isolate the slurry of the slurries of the containing ammonium chloride solid on upper layer and the sulfur acid potassium ammonium of lower layer, potassium sulfate solid；S3: the slurry of sulfur acid potassium ammonium, potassium sulfate solid is separated by solid-liquid separation, and liquid phase is mother liquor 2, and solid phase potassium-ammonium sulfate and potassium sulfate are admitted to converter, and converter is added in saturated potassium chloride solution and react forming potassium sulfate with potassium-ammonium sulfate.The present invention prepares potassium product of the potassium oxide mass percentage 50% or more by gravity selection separation and secondary conversion, avoids reducing evaporation capacity, technically simple, condition is easily-controllable, at low cost using catalyst.
Description
Technical field
The present invention relates to a kind of preparation methods of potassium sulfate, and especially a kind of is at normal temperature original with potassium chloride and ammonium sulfate
The double decomposition of material prepares the preparation system and method for high-recovery potassium sulfate.
Background technique
Potassium sulfate is a kind of important no high-quality potash fertilizer of chlorine, and potassium element is one of plant three nutritious elements, and sulphur is plant institute
The middle amount nutrient needed.It is more suitable compared with potassium chloride for avoiding chlorine industrial crops potassium sulfate for such as tobacco, citrus, tealeaves, sugarcane etc.
The multiplicity of conjunction is divided booty material, and applying range and effect will get well more than potassium chloride.In addition, potassium sulfate is also a kind of basic chemical industry raw material,
It is widely used in medicine, glass and dye industry.Potassium sulfate annual requirement in China's is at 1,000,000 tons or more at present, domestic sulfuric acid
Potassium total output is far below demand, and potassium sulfate relies heavily on import.
Currently, the method for domestic production potassium sulfate mainly has potassium ore comprehensive use, bittern comprehensive use, Mannheim
The double decomposition of method and sulfate and potassium chloride.Wherein, potassium ore comprehensive use and bittern comprehensive use are because resource has
Limit cannot be widely used, and Mannheim rule is due to investing the originals such as big, energy consumption height, equipment seriously corroded, by-product slack market
Because also restrained.Therefore, the production technology of potassium sulfate is researched and developed, there is certain realistic meaning.
The method produced by sulfate and potassium chloride double decomposition, with stronger excellent from economic and social benefit
Gesture, therefore increasingly attract everybody sight.
First high temperature saturated solution is respectively prepared in potassium chloride, ammonium sulfate by Chinese patent CN1168350A proposition, then by two
The mixing of kind of solution goes out major product potassium sulfate using decrease temperature crystalline, and filtrate evaporation goes water to obtain byproduct ammonium chloride, but potassium
Conversion ratio only has 70%, and evaporation energy consumption is high, quality less stable.
Chinese patent CN104386713A proposition mixes ammonium sulfate, potassium chloride, circulating mother liquor, cleaning solution under certain condition
Reaction is closed, thick potassium sulfate is obtained by filtration, thick potassium sulfate obtains product potassium sulfate through water washing.It is washed out after the crystallization of filtrate cooling down
Ammonium chloride, mother liquor and cleaning solution after ammonium chloride is precipitated, which return, to be recycled.This process product potassium sulfate is unable to reach high-class product
Standard, and potassium conversion ratio is less than 75%, can not widely apply and industrial production.
Chinese patent CN1086178A proposes that reaction is mixed with potassium chloride, ammonium sulfate saturated solution, rear to be added again
NH4HCO3, thick potassium sulfate is obtained by filtration, Klorvess Liquid secondary response is added in thick potassium sulfate, is separated by filtration to obtain through sulfuric acid
Potassium.Good product quality, potassium utilization rate are high.But since catalyst KOH being added in the process, caused catalyst enrichment and recycling are asked
Topic, is unfavorable for industrial production.
Chinese patent CN104386713A is proposed to be stirred at a certain temperature in proportion with potassium mother liquor and ammonium sulfate, is settled and divide
Ammonium potassium clear liquid and slurry are separated out, ammonium chloride potassium by-product and ammonium mother liquor are isolated in the evaporation of ammonium potassium clear liquid, with slurry after the heating of ammonium mother liquor
Material and potassium sulfate wash and starch liquid and are mixed in a certain ratio and are added potassium chloride secondary response, sedimentation, obtain thick potassium sulfate slurries, then
Secondary washing obtains potassium product again after being wherein centrifugated after the washing of addition potassium washing lotion.This process needs to be heated at high temperature, energy consumption
Greatly, and high temperature corrosion requires height to equipment and materials, therefore less economical.
To solve the above problems, the present invention proposes that a kind of process is simple, energy consumption is lower, and product grade is high, convenient for industrialization
Room temperature double decomposition conversion preparing potassium sulfate new process.
Summary of the invention
To solve drawbacks described above, the present invention provides a kind of preparation method of potassium sulfate, a kind of preparation method of potassium sulfate, packet
It includes following steps: S1: ammonium sulfate being added in salt dissolving groove to the solution for being configured to ammonium sulfate concentrations and reaching saturation, then by describedization
Solution in salt bath is introduced into crystallizer, and solid potassium chloride is added in the crystallizer and react simultaneously shape with the solution
At crystallization；S2: the solution after reacting in S1 step and crystal are subjected to Gravity Separation, isolate the containing ammonium chloride solid on upper layer
Slurries and the sulfur acid potassium ammonium of lower layer, potassium sulfate solid slurry；S3: by the sulfur acid potassium ammonium, the material of potassium sulfate solid
Slurry is separated by solid-liquid separation, and liquid phase is mother liquor 2, and solid phase potassium-ammonium sulfate and potassium sulfate are admitted to converter, by saturated potassium chloride solution
The converter is added react forming potassium sulfate with the potassium-ammonium sulfate.
According to an embodiment of the present invention, further including in the S1 step will be described in the solution introducing in the salt dissolving groove
Step is filtered to the solution before crystallizer.
Another embodiment according to the present invention, further includes step S4: the containing ammonium chloride generated in S2 step is consolidated
The slurries of body are separated by solid-liquid separation, and liquid phase is mother liquor 1, and solid phase is ammonium chloride.
Another embodiment according to the present invention, further includes step S5: potassium sulfate prepared by S3 step being washed, is washed
Solution after washing is back to the salt dissolving groove.
Another embodiment according to the present invention, further includes step S6: the mother liquor 1 and the mother liquor 2 are introduced respectively
To evaporator, it is concentrated by evaporation in the evaporator and forms concentrated mother liquor, the concentrated mother liquor is back to the salt dissolving groove；Evaporation
The condensed water of generation is used for the washing of S5 step.
Another embodiment according to the present invention further includes being separated by solid-liquid separation the slurry after S3 step reaction, liquid phase
It is back to the salt dissolving groove, solid phase is dried, cooling step.
The present invention also provides a kind of preparation systems of potassium sulfate, comprising: primary first-order equation unit, for ammonium sulfate concentrations to be reached
Solution to saturation is reacted with solid potassium chloride and forms crystallization；Gravity Separation unit is used for the primary first-order equation list
The solution and crystal reacted in member isolates the slurries of the containing ammonium chloride solid on upper layer and sulfur acid potassium ammonium, the sulphur of lower layer
The slurry of sour potassium solid；Secondary conversion unit, for the slurry of the sulfur acid potassium ammonium, potassium sulfate solid to be carried out solid-liquid point
From, and potassium-ammonium sulfate in solid phase react forming potassium sulfate with saturated potassium chloride solution.
According to an embodiment of the present invention, the preparation system of the potassium sulfate further includes upgrading unit, for will be through
The containing ammonium chloride solid slurry after Gravity Separation unit separation be separated by solid-liquid separation after liquid phase and the secondary conversion list
Liquid phase is concentrated by evaporation to form concentrated mother liquor after the slurry of the sulfur acid potassium ammonium, potassium sulfate solid in member is separated by solid-liquid separation,
The concentrated mother liquor is back to the primary first-order equation unit.
Another embodiment according to the present invention, the preparation system of the potassium sulfate further includes drying unit, for doing
The potassium sulfate that the dry secondary conversion unit is formed.
Another embodiment according to the present invention, the drying unit include deduster, are generated for recycling drying process
Dust.
The present invention by gravity selection separation and secondary conversion preparation the mass percentage in terms of potassium oxide 50% with
On potassium product, avoid reducing evaporation capacity, technically simple, condition is easily-controllable, at low cost using catalyst.Meanwhile passing through weight
Power separation can also realize that by-product ammonium chloride high-purity separates.Further, mother liquor concentrations in the process recycle, and save
Cost reduces the harm to environment.
Detailed description of the invention
Fig. 1 is the process flow diagram of double decomposition preparing potassium sulfate of the present invention.
Specific embodiment
It elaborates With reference to embodiment to the present invention.
Embodiment 1
Primary first-order equation is carried out in primary first-order equation unit.At normal temperature, ammonium sulfate solids are added in salt dissolving groove to be dissolved with water,
After incorporation time 20min, it is configured to the solution that ammonium sulfate concentrations reach saturation, is filtered to remove insoluble matter.With ammonium sulfate and chlorination
The molar ratio of potassium is the ratio of 1:0.9, ammonium sulfate saturated solution and technical grade solid potassium chloride is added anti-in reaction crystalizer
It should and crystallize, the reactive crystallization time is 20min, and potassium chloride in ammonium sulfate sufficiently complete by reaction, and slurries are standby in reactor
With.Yield of this process potassium sulfate is 90%.
By the slurries (solid content 17%) of primary first-order equation unit through being pumped into Gravity Separation unit, through Gravity Separation unit
Gravity separator carry out Gravity Separation, gravity separator top exit discharging be ammonium chloride slurry, bottom discharge be containing solid phase
The slurries of potassium-ammonium sulfate and potassium sulfate, yield of this process potassium sulfate is 95% or more.
By the slurries of the potassium-ammonium sulfate containing solid phase of gravity separator bottom discharge and potassium sulfate in secondary conversion unit into
Row centrifuge separation, isolated liquid phase are mother liquor 2, the micro- wet stock potassium-ammonium sulfate of solid phase, potassium sulfate (water content≤8%).It will be micro- wet
Object is sent into converter, and saturated potassium chloride solution is added and carries out secondary conversion, converts thick potassium sulfate for potassium-ammonium sulfate.It then will be thick
Potassium sulfate slurry centrifuge separation, liquid phase is mother liquor 3, and the thick potassium sulfate of solid phase (water content≤8%) is spare, this process potassium sulfate is once received
95% or more rate.
The thick potassium sulfate prepared in secondary conversion unit is sent into washing tank and carries out pulp washing, adjusts solids in pulp amount
It is 20% or so, then wash time 15min is centrifuged, filtrate is mother liquor 4, wet stock potassium sulfate (water content
≤ 8%) spare, 85% or more yield of this process potassium sulfate.
The slurries for the containing ammonium chloride solid expected at gravity separator top exit are separated by solid-liquid separation, liquid phase is mother liquor 1,
Solid phase is wet feed ammonium chloride.
The excessively middle mother liquor 1 generated of above-mentioned mistake and mother liquor 2 are concentrated by evaporation in the evaporator of evaporation element, then carried out cold
But.Condensed water is dense for preparing saturated potassium chloride solution and the washing to the wet stock potassium sulfate prepared in secondary conversion unit
Concentrated mother liquor, mother liquor 3 and partial mother liquid 4 after contracting are back to ammonium sulfate salt dissolving groove.
Wet stock potassium sulfate after washing enters drying unit, dry by rotary-drum drier, defeated by bucket elevator
It send to feed bin, the potassium sulfate dust of dryer export enters feed bin, this process by cyclone dust collectors and sack cleaner processing heel row
98% or more yield of potassium sulfate.
Wet feed ammonium chloride (water content≤11%) is dry into rotary-drum drier, is delivered to feed bin by bucket elevator,
The potassium sulfate dust of dryer export enters feed bin by cyclone dust collectors and sack cleaner processing heel row.
Dry hot wind used brings drying cylinder by heat exchanger, air blower and air-introduced machine by hot blast stove system burning char particle
In.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (10)
1. a kind of preparation method of potassium sulfate, which comprises the steps of:
Ammonium sulfate: being added in salt dissolving groove the solution for being configured to ammonium sulfate concentrations and reaching saturation by S1, then will be in the salt dissolving groove
Solution be introduced into crystallizer, and solid potassium chloride is added and is reacted and formed knot in the crystallizer with the solution
It is brilliant；
S2: the solution after reacting in S1 step and crystal are subjected to Gravity Separation, isolate the containing ammonium chloride solid on upper layer
The slurry of slurries and the sulfur acid potassium ammonium of lower layer, potassium sulfate solid；
S3: the slurry of the sulfur acid potassium ammonium, potassium sulfate solid is separated by solid-liquid separation, and liquid phase is mother liquor 2, solid phase potassium-ammonium sulfate
It is admitted to converter with potassium sulfate, the converter is added in saturated potassium chloride solution and carries out reacting formation with the potassium-ammonium sulfate
Potassium sulfate.
2. the preparation method of potassium sulfate according to claim 1, which is characterized in that further including in the S1 step will be described
Solution in salt dissolving groove is filtered step to the solution before introducing the crystallizer.
3. the preparation method of potassium sulfate according to claim 1, which is characterized in that further include step
S4: the slurries of the containing ammonium chloride solid generated in S2 step are separated by solid-liquid separation, and liquid phase is mother liquor 1, and solid phase is
Ammonium chloride.
4. the preparation method of potassium sulfate according to claim 1, which is characterized in that further include step
S5: potassium sulfate prepared by S3 step is washed, and the solution after washing is back to the salt dissolving groove.
5. the preparation method of potassium sulfate according to claim 4, which is characterized in that further include step
S6: being introduced separately to evaporator for the mother liquor 1 and the mother liquor 2, is concentrated by evaporation in the evaporator and forms concentration
Mother liquor, the concentrated mother liquor are back to the salt dissolving groove；The condensed water that evaporation generates is used for the washing of S5 step.
6. the preparation method of potassium sulfate according to claim 1, which is characterized in that further include by the slurry after S3 step reaction
Material is separated by solid-liquid separation, and liquid phase is back to the salt dissolving groove, and solid phase is dried, cooling step.
7. a kind of preparation system of potassium sulfate characterized by comprising
Primary first-order equation unit, the solution for ammonium sulfate concentrations to be reached to saturation are reacted with solid potassium chloride and form knot
It is brilliant；
Gravity Separation unit, for the solution and crystal that react in the primary first-order equation unit to be isolated containing for upper layer
The slurry of the slurries of chloride solid and the sulfur acid potassium ammonium of lower layer, potassium sulfate solid；
Secondary conversion unit, for the slurry of the sulfur acid potassium ammonium, potassium sulfate solid to be separated by solid-liquid separation, and will be in solid phase
Potassium-ammonium sulfate react forming potassium sulfate with saturated potassium chloride solution.
8. the preparation system of potassium sulfate according to claim 7, which is characterized in that further include upgrading unit, being used for will be through described
In the liquid phase and the secondary conversion unit after containing ammonium chloride solid slurry separation of solid and liquid after the separation of Gravity Separation unit
The sulfur acid potassium ammonium, potassium sulfate solid slurry be separated by solid-liquid separation after liquid phase be concentrated by evaporation to form concentrated mother liquor, it is described
Concentrated mother liquor is back to the primary first-order equation unit.
9. the preparation system of potassium sulfate according to claim 7, which is characterized in that further include drying unit, described in dry
The potassium sulfate that secondary conversion unit is formed.
10. the preparation system of potassium sulfate according to claim 9, which is characterized in that the drying unit includes deduster, is used for
Recycle the dust that drying process generates.
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| CN201711329164.9A CN109911919A (en) | 2017-12-13 | 2017-12-13 | Potassium sulfate preparation system and method |
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| CN201711329164.9A CN109911919A (en) | 2017-12-13 | 2017-12-13 | Potassium sulfate preparation system and method |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1098702A (en) * | 1993-08-13 | 1995-02-15 | 贵州工学院化工厂 | Production of potashsium sulfate with assistant method |
| CN1129684A (en) * | 1995-02-22 | 1996-08-28 | 四川联合大学 | Combinating process for producing ammonium-potassium sulfate and nitrogen-phosphorus-potassium composite fertilizer |
| CN1220249A (en) * | 1998-08-05 | 1999-06-23 | 重庆菲尔达技术公司 | Method for preparing potassium sulfate by double conversion of ammonium sulfate |
| WO1999065823A1 (en) * | 1998-06-16 | 1999-12-23 | Airborne Industrial Minerals Inc. | Method of procucing potassium sulfate |
| CN1290655A (en) * | 1999-09-30 | 2001-04-11 | 邓杰华 | Gravity separation method for producing potassium sulfate |
| CN106315627A (en) * | 2016-08-12 | 2017-01-11 | 宜昌富升化工有限公司 | Production technology of potassium sulfate |
| CN106467311A (en) * | 2015-08-17 | 2017-03-01 | 吴有章 | Method using waster KCl production full water-soluble potassium sulfate |
-
2017
- 2017-12-13 CN CN201711329164.9A patent/CN109911919A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1098702A (en) * | 1993-08-13 | 1995-02-15 | 贵州工学院化工厂 | Production of potashsium sulfate with assistant method |
| CN1129684A (en) * | 1995-02-22 | 1996-08-28 | 四川联合大学 | Combinating process for producing ammonium-potassium sulfate and nitrogen-phosphorus-potassium composite fertilizer |
| WO1999065823A1 (en) * | 1998-06-16 | 1999-12-23 | Airborne Industrial Minerals Inc. | Method of procucing potassium sulfate |
| CN1220249A (en) * | 1998-08-05 | 1999-06-23 | 重庆菲尔达技术公司 | Method for preparing potassium sulfate by double conversion of ammonium sulfate |
| CN1290655A (en) * | 1999-09-30 | 2001-04-11 | 邓杰华 | Gravity separation method for producing potassium sulfate |
| CN106467311A (en) * | 2015-08-17 | 2017-03-01 | 吴有章 | Method using waster KCl production full water-soluble potassium sulfate |
| CN106315627A (en) * | 2016-08-12 | 2017-01-11 | 宜昌富升化工有限公司 | Production technology of potassium sulfate |
Non-Patent Citations (1)
| Title |
|---|
| 张罡等: "硫酸铵转化法制取硫酸钾新工艺", 《海湖盐与化工》 * |
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