CN106315627A - Production technology of potassium sulfate - Google Patents
Production technology of potassium sulfate Download PDFInfo
- Publication number
- CN106315627A CN106315627A CN201610660088.9A CN201610660088A CN106315627A CN 106315627 A CN106315627 A CN 106315627A CN 201610660088 A CN201610660088 A CN 201610660088A CN 106315627 A CN106315627 A CN 106315627A
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- Prior art keywords
- potassium
- potassium sulfate
- sulfate
- mother solution
- ammonium
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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
Abstract
The invention provides a production technology of potassium sulfate. The production technology comprises the following steps that ammonium sulfate is dissolved with mother liquor II and condensation water and then fed into a mixing reactor; potassium chloride is added into the mixing reactor, and slurry obtained after ammonium sulfate liquor and potassium chloride are fully mixed and react is centrifuged, filtered and separated to obtain mother liquor I and crude potassium sulfate; the mother liquor I is subjected to concentration, cooling crystallization and centrifugal separation to obtain potassium ammonium chloride and mother liquor III; the mother liquor III is fed into a concentration work section to be cyclically used, one part of condensation water generated through concentration is used for dissolving ammonium sulfate, and the other part of condensation water is cooled by a heat exchanger and then used for washing a crude potassium sulfate product, and the crude potassium sulfate product obtained after washing is subjected to centrifugal separation and drying to obtain the potassium sulfate product and the mother liquor II. According to the method, the adopted raw materials are cheap and easy to obtain, and therefore the production cost is low; in addition, the whole production technology is totally closed and cyclic, three wastes are not generated, and therefore the technology is a pure green technology.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of method producing potassium sulfate, specially one utilizes ammonium sulfate
Method with KCl production potassium sulfate.
Background technology
Potassium sulfate, as a kind of important potash fertilizer of high-quality without chlorine, contains again the element sulphur required for crops, extensively simultaneously
Applying in agricultural production, such as Nicotiana tabacum L., Citrus, Folium Camelliae sinensis, Fructus Vitis viniferae, Radix Betae etc., it not only can improve agricultural product quality, moreover it is possible to improves
Its quality.But potassium salt is a kind of non-renewable resources, and the distributed pole in the whole world is uneven, and the most Canadian and former Soviet Union divides
The 40% and 37% of Bie Zhan world potassium salt total resources.
Along with the development of agricultural, the demand of potassium salt is incremented by by China every year constantly, and huge demand gap, for potassium salt
Market provides wide prospect.At present, supply falls short of demand for whole world potassium salt, and price rises steadily.But potassium salt especially high-quality sulfur
The production technology of acid potassium is not disclosed always, how to utilize ammonium sulfate, KCl production high-quality, the potassium sulfate of low cost to be stranded always
Disturb Chemical Manufacture enterprise.At present, ammonium sulfate, the method for KCl production potassium sulfate is utilized to have several, Deutsche Bundespatent
Ger.offen2142114(1973) be utilized in excess 5-10%(mole) ammonium sulfate in add solid potassium chloride not
Disconnected stirring, makes in suspended state, i.e. has a large amount of potassium sulfate to crystallize out, then until satisfying in 15-40 DEG C of logical ammonia to aaerosol solution
With, make to crystallize out further potassium sulfate, isolate the solution evaporation after potassium sulfate and go out ammonia, recycle.Evaporate and cool down and stay
Solution obtain ammonium chloride.In this technique, potassium sulfate crystallizes in the saturated solution of ammonia and separates, to improving product potassium sulfate
Purity is favourable, but because using ammonia to circulate in production technology, recovery ammonia equipment to be increased makes flow process complicate, and also can not keep away
To consume a number of ammonia with exempting from, and production operation environment and health and safety condition will be made to deteriorate.Japanese patent gazette
Clear 48-22907 is to use NH4/ K=1(mol ratio) 28.25% ammonium sulfate in add below 100 DEG C potassium chloride stirring
Reacting 10 DEG C of crystallizations, fraction of 50% methanol aqueous solution of crude product liquid containing ammonium sulfate processes, and mother solution again with methanol processes and reclaims sulphuric acid
Potassium, obtains product containing K2O 53-53.6%, K2The O response rate more than 90%, but use poisonous methanol to process, inclement condition.Specially
The profit potassium dihydrogen phosphate of Application No. 89106858.9, the production method of potassium sulfate and the nitric acid of Application No. 90105324.4
Potassium, potassium dihydrogen phosphate, potassium sulfate production method in disclose the production method of a kind of potassium sulfate, its method is that first preparation contains
The circulation solution of sodium nitrate, heats this circulation solution and fertilizer potassium chloride effect precipitated sodium chloride, the mother solution after Isolating chlorinated sodium
Cool precipitation potassium chloride, and the mother solution after Isolating chlorinated potassium produces potassium sulfate with ammonium sulfate effect, and Recycling Mother Solution uses, at this
In method, need first to make intermedium, prepare potassium sulfate, complex technical process by intermedium the most again.
It is an object of the invention to provide a kind of with ammonium sulfate, potassium chloride as raw material, raw for solvent with mother solution and condensed water
Produce the process of potassium sulfate, be possible not only to stably produce high-class product potassium sulfate, and can obtain directly using
Side-product ammonium chloride potassium, meanwhile, whole technical process is the most simple, and produces without any three wastes, during produce mother
Liquid, condensed water etc. are all recycled.
Summary of the invention
It is an object of the invention to for problem above, it is provided that a kind of side utilizing ammonium sulfate and KCl production potassium sulfate
Method, it is possible to use cheap raw material to produce higher quality potassium sulfate.
The technical solution adopted in the present invention is: a kind of process for producing potassium sulfate, specifically comprises the following steps that
(1) ammonium sulfate is added mother solution and condensed water in dissolving tank wiring solution-forming send into hybrid reaction groove, then press ammonium sulfate and
The amount that reaction mol ratio is 1:1.5 ~ 1:3 of potassium chloride adds potassium chloride in hybrid reaction groove, and the two is sufficiently mixed reaction, instead
Temperature is answered to control 40-80 DEG C, response time 0.1-3h.
(2) it is centrifuged step (1) gained reaction slurry filtering separating, obtains thick product potassium sulfate and mother solution I.
(3) by the thick potassium sulfate of step (2) gained through being proportionally added into particular solution purification, being centrifugally separating to obtain sulphuric acid
Potassium and mother solution II, potassium sulfate the most i.e. can get the mass ratio control of product potassium sulfate, particular solution consumption and thick potassium sulfate
It is made as 0.5-2:1.
(4) by the mother solution I of step (2) gained again through being concentrated into crystallisation by cooling after proportion is about 1.2-1.40g/ml,
Centrifugal filtration obtains mother solution III and crude product ammonium chloride potassium, the dry by-product ammonium chloride potassium that i.e. can get, the control of crystallisation by cooling temperature
At 20-70 DEG C.
(5) mother solution II in step (3) is cycled to used in the dissolving of ammonium sulfate in step (1), can fully improve raw material
Utilization rate.
(6) mother solution III in step 4) is returned to the concentration section in step 4) and is circulated utilization, improve ammonium chloride
Potassium yield.
(7) condensation water collection obtained after the mother solution III in step (4) and mother solution 1 being concentrated, after filling into fresh water (FW)
A part is used in step (1) dissolving ammonium sulfate, and another part is used for the purification of thick product potassium sulfate after heat exchanger heat exchange.
The method have the advantages that
1, produce raw material and use the ammonium sulfate of company's by-product and potassium chloride cheap and easy to get, considerably reduce and produce into
This.In current society, potassium sulfate price is at about 2900 yuan/ton.This technique produces 1 ton of potassium sulfate, consumes ammonium sulfate about
0.75 ton, about 0.85 ton of potassium chloride, equivalent cost about 2500 yuan；Generate about 0.5 ton of ammonium chloride potassium (butt) simultaneously, can
Cost-recovering about about 500 yuan, profit is considerable.
2, whole production technology closed circulating produces, and produces without any three wastes, sheerly friendly process.
3, this production technology device is simple, and easy to operate, process conditions are easily controllable, good product quality, consume low, and potassium is received
Rate reaches more than 90%.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the present invention.
Detailed description of the invention
Further illustrate the present invention below in conjunction with case study on implementation and accompanying drawing, but case study on implementation will not be constituted the present invention's
Limit.
Implement 1: be dissolved in water in reactive tank by ammonium sulfate, then add and ammonium sulfate mol ratio 1:1.5 in reactive tank
Potassium chloride, control reaction temperature 65 DEG C, in the case of being sufficiently stirred for react 1h, reacted slip machine by centrifugation separate,
Obtain thick potassium sulfate and mother solution I, in thick potassium sulfate, add the water with thick potassium sulfate mass ratio 0.5:1 after purification, enter centrifugal
Machine centrifugation, obtains product potassium sulfate and mother solution II, and the mother solution I obtained enters enrichment facility and is concentrated into proportion is 1.4g/ml,
It is cooled to 30 DEG C of crystallizations, then is performing centrifugal separation on obtaining mother solution III and ammonium chloride potassium, be dried and i.e. can get by-product ammonium chloride potassium,
It is interior for dissolving ammonium sulfate that mother solution II returns reactive tank, and mother solution III then returns concentration section and recycles.
In the potassium sulfate obtained, potassium oxide content is 50.2%.
Implement 2: be dissolved in water in reactive tank by ammonium sulfate, then add in reactive tank and ammonium sulfate mol ratio 1:2
Potassium chloride, controls reaction temperature 80 DEG C, reacts 1.5h in the case of being sufficiently stirred for, and reacted slip machine by centrifugation separates,
Obtain thick potassium sulfate and mother solution I, in thick potassium sulfate, add the water with thick potassium sulfate mass ratio 1:1 after purification, enter centrifuge
Centrifugation, obtains product potassium sulfate and mother solution II, and the mother solution I obtained enters enrichment facility and is concentrated into proportion is 1.35g/ml,
It is cooled to 30 DEG C of crystallizations, then is performing centrifugal separation on obtaining mother solution III and ammonium chloride potassium, be dried and i.e. can get by-product ammonium chloride potassium,
It is interior for dissolving ammonium sulfate that mother solution II returns reactive tank, and mother solution III then returns concentration section and recycles.
In the potassium sulfate obtained, potassium oxide content is 50.8%.
Implement 3: be dissolved in water in reactive tank by ammonium sulfate, then add in reactive tank and ammonium sulfate mol ratio 1:2
Potassium chloride, controls reaction temperature 65 DEG C, reacts 1h in the case of being sufficiently stirred for, and reacted slip machine by centrifugation separates,
To thick potassium sulfate and mother solution I, in thick potassium sulfate, add the water with thick potassium sulfate mass ratio 1.2:1 after purification, enter centrifuge
Centrifugation, obtains product potassium sulfate and mother solution II, and the mother solution I obtained enters enrichment facility and is concentrated into proportion is 1.4g/ml, then
It is cooled to 30 DEG C of crystallizations, then is performing centrifugal separation on obtaining mother solution III and ammonium chloride potassium, be dried and i.e. can get by-product ammonium chloride potassium, female
It is interior for dissolving ammonium sulfate that liquid II returns reactive tank, and mother solution III then returns concentration section and recycles.
In the potassium sulfate obtained, potassium oxide content is 51.3%.
Claims (8)
1. a process for producing potassium sulfate, it is characterised in that: include following process:
(1) ammonium sulfate is added mother solution and condensed water wiring solution-forming in dissolving tank and sends into hybrid reaction groove, then according to ammonium sulfate
Adding potassium chloride in hybrid reaction groove with the mol ratio of potassium chloride, the two is sufficiently mixed reaction, controls reaction temperature, during reaction
Between；
(2) it is centrifuged step (1) gained reaction slurry filtering separating, obtains thick product potassium sulfate and mother solution I；
(3) the thick potassium sulfate of step (2) gained is proportionally added into particular solution purification, is centrifugally separating to obtain potassium sulfate and mother solution
II, potassium sulfate the most i.e. can get product potassium sulfate；
(4) by the mother solution I of step (2) gained again after being concentrated into certain weight proportion crystallisation by cooling, centrifugal filtration obtain mother solution III
With crude product ammonium chloride potassium, be dried i.e. can get by-product ammonium chloride potassium；
(5) mother solution II in step (3) is cycled to used in the dissolving of ammonium sulfate in step (1), can fully improve raw material and utilize
Rate；
(6) mother solution III in step (4) is returned to the concentration section in step (4) and is circulated utilization, improve ammonium chloride potassium
Yield；
(7) will the mother solution III in step (4) and mother solution I concentrate after the condensation water collection that obtains, fill into after fresh water (FW) one
Dividing and be used in step (1) dissolving ammonium sulfate, another part is used for the washing purification of thick product potassium sulfate after heat exchanger heat exchange.
The production technology of potassium sulfate the most according to claim 1, it is characterised in that: the dissolving sulphuric acid described in step (1)
Solvent used by ammonium is that mother solution I and mother solution III concentrates condensed water and mother solution II, if quantity of solvent can be cold time inadequate in the reaction of this step
Solidifying tank fills into one-time process water.
The production technology of potassium sulfate the most according to claim 1, it is characterised in that: the ammonium sulfate described in step (1) with
The reaction mol ratio of potassium chloride is 1:1 ~ 1:3.
The production technology of potassium sulfate the most according to claim 1, it is characterised in that: the ammonium sulfate described in step (1) with
The reaction temperature of potassium chloride is 40-80 DEG C, and the response time is 0.1-3 h.
The production technology of potassium sulfate the most according to claim 1, it is characterised in that: for potassium sulfate described in step (3)
The particular solution of purification is water or the solution of potassium sulfate or the saturated solution of potassium sulfate, and its consumption with the mass ratio of thick potassium sulfate is
0.5~2:1。
The production technology of potassium sulfate the most according to claim 1, it is characterised in that: the ammonium sulfate described in step (3) with
After potassium chloride reaction, to be further concentrated to proportion through the mother solution I being centrifugally separating to obtain be 1.2-1.4g/ml, cooled crystallization, centrifugal
Be filtrated to get mother solution III, be dried i.e. can get side product chlorinated ammonia potassium, crystallisation by cooling temperature controls at 20-70 DEG C.
The production technology of potassium sulfate the most according to claim 6, it is characterised in that: mother solution III again returns to concentrator circulation
Utilize.
The production technology of potassium sulfate the most according to claim 6, it is characterised in that: mother solution III and mother solution I concentrated after
To water condensate storage in condensate draining, a part be used for the first step dissolve ammonium sulfate, another part through heat exchanger lower the temperature
After be used for the purification of thick product potassium sulfate, one-time process water can be filled into time not enough in condensate draining.
Priority Applications (1)
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| CN201610660088.9A CN106315627A (en) | 2016-08-12 | 2016-08-12 | Production technology of potassium sulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417307A (en) * | 2017-09-12 | 2017-12-01 | 化工部长沙设计研究院 | A kind of preparation technology of water-soluble drip irrigation potassium sulfate |
| CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
| CN111520975A (en) * | 2020-06-02 | 2020-08-11 | 湖南省湘衡盐化有限责任公司 | Industrial salt drying system and method |
| CN111606335A (en) * | 2020-05-27 | 2020-09-01 | 天宝动物营养科技股份有限公司 | Method for comprehensively utilizing clean potassium salt-containing mother liquor |
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| 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 |
| CN1166453A (en) * | 1997-05-09 | 1997-12-03 | 郑州工业大学 | Combiend production process of potassium carbonate and light magnesium carbonate |
| CN1218005A (en) * | 1997-11-21 | 1999-06-02 | 烟台中兴化工有限公司 | Method for preparation of potassium sulfate |
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| CN1299337A (en) * | 1998-06-16 | 2001-06-13 | 艾尔伯恩工业矿物公司 | Method of producing potassium sulfate |
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| CN105540616A (en) * | 2015-12-21 | 2016-05-04 | 太原科技大学 | Method for preparing potassium sulfate by double-decomposition closed-cycle process |
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Patent Citations (7)
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| 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 |
| CN1166453A (en) * | 1997-05-09 | 1997-12-03 | 郑州工业大学 | Combiend production process of potassium carbonate and light magnesium carbonate |
| CN1218005A (en) * | 1997-11-21 | 1999-06-02 | 烟台中兴化工有限公司 | Method for preparation of potassium sulfate |
| CN1299337A (en) * | 1998-06-16 | 2001-06-13 | 艾尔伯恩工业矿物公司 | Method of producing potassium sulfate |
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| CN1336323A (en) * | 2000-08-02 | 2002-02-20 | 山东新华工贸股份有限公司 | Method and equipment of preparing potassium sulfate and ammonium potassium chloride with industrial effluent containing ammonium sulfate |
| CN105540616A (en) * | 2015-12-21 | 2016-05-04 | 太原科技大学 | Method for preparing potassium sulfate by double-decomposition closed-cycle process |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417307A (en) * | 2017-09-12 | 2017-12-01 | 化工部长沙设计研究院 | A kind of preparation technology of water-soluble drip irrigation potassium sulfate |
| CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
| CN111606335A (en) * | 2020-05-27 | 2020-09-01 | 天宝动物营养科技股份有限公司 | Method for comprehensively utilizing clean potassium salt-containing mother liquor |
| CN111520975A (en) * | 2020-06-02 | 2020-08-11 | 湖南省湘衡盐化有限责任公司 | Industrial salt drying system and method |
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