CN106044802A - Fully water-soluble crystal potassium sulfate production process - Google Patents
Fully water-soluble crystal potassium sulfate production process Download PDFInfo
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- CN106044802A CN106044802A CN201610667990.3A CN201610667990A CN106044802A CN 106044802 A CN106044802 A CN 106044802A CN 201610667990 A CN201610667990 A CN 201610667990A CN 106044802 A CN106044802 A CN 106044802A
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- Prior art keywords
- potassium sulfate
- potassium
- raw material
- soluble
- watersoluble
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- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title claims abstract description 144
- 229910052939 potassium sulfate Inorganic materials 0.000 title claims abstract description 142
- 235000011151 potassium sulphates Nutrition 0.000 title claims abstract description 142
- 239000013078 crystal Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 53
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000011591 potassium Substances 0.000 claims abstract description 43
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000012267 brine Substances 0.000 claims abstract description 12
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000001117 sulphuric acid Substances 0.000 claims description 12
- 235000011149 sulphuric acid Nutrition 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- -1 2-ethylhexyl Chemical group 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 4
- ILRLTAZWFOQHRT-UHFFFAOYSA-N potassium;sulfuric acid Chemical compound [K].OS(O)(=O)=O ILRLTAZWFOQHRT-UHFFFAOYSA-N 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- NLNXYXXHVONUCN-UHFFFAOYSA-N 2-ethylhexylphosphane Chemical compound CCCCC(CC)CP NLNXYXXHVONUCN-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 238000005202 decontamination Methods 0.000 claims 1
- 230000003588 decontaminative effect Effects 0.000 claims 1
- 239000003337 fertilizer Substances 0.000 abstract description 22
- 238000003973 irrigation Methods 0.000 abstract description 14
- 230000002262 irrigation Effects 0.000 abstract description 14
- 230000008025 crystallization Effects 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000007921 spray Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 21
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 241001131796 Botaurus stellaris Species 0.000 description 6
- 239000001103 potassium chloride Substances 0.000 description 6
- 235000011164 potassium chloride Nutrition 0.000 description 6
- JJJOZVFVARQUJV-UHFFFAOYSA-N 2-ethylhexylphosphonic acid Chemical class CCCCC(CC)CP(O)(O)=O JJJOZVFVARQUJV-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229940072033 potash Drugs 0.000 description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 5
- 235000015320 potassium carbonate Nutrition 0.000 description 5
- 235000002639 sodium chloride Nutrition 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000001120 potassium sulphate Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000012271 agricultural production Methods 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 235000011128 aluminium sulphate Nutrition 0.000 description 1
- 229910052934 alunite Inorganic materials 0.000 description 1
- 239000010424 alunite Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 description 1
- 230000001228 trophic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C01D5/16—Purification
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
- C05D1/02—Manufacture from potassium chloride or sulfate or double or mixed salts thereof
-
- 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
-
- 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
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a fully water-soluble potassium sulfate production process comprising the following steps: (1) preparing a first fully water-soluble potassium sulfate intermediate raw material: preparing potassium sulfate by using a potassium sulfate ore or potassium-containing brine; and preparing a second fully water-soluble potassium sulfate intermediate raw material: preparing potassium sulfate by using Mannheim process; (2) mixing the first fully water-soluble potassium sulfate intermediate raw material and the second fully water-soluble potassium sulfate intermediate raw material, dissolving, extracting, and filtering to remove impurities, to obtain a potassium sulfate intermediate solution; and (3) carrying out cooling crystallization of the potassium sulfate intermediate solution, and thus obtaining fully water-soluble potassium sulfate. According to the fully water-soluble potassium sulfate production process, with combination of two different potassium sulfate raw material preparation schemes in the prior art, the potassium sulfate production technological route in the prior art can be directly combined in the preparation process of the fully water-soluble potassium sulfate, the upgrading and reconstruction process is gentle, the reconstruction cost is low, the economic benefits of enterprises are facilitated to be improved, moreover, the potassium sulfate product has uniform and coarse crystals, is fully soluble in water, and can be used as spray and drop irrigation fertilizers.
Description
Technical field
The present invention relates to a kind of process for producing potassium sulfate, particularly to the process for producing potassium sulfate of a kind of full water-soluble, belong to
In chemical field potash fertilizer process technology.
Background technology
Potash fertilizer is one of required three big trophic factors of crop growthing development, multiple in potassium element direct involved in plant body
The activity of enzyme, if plant lacks potash fertilizer, then the transport of plant substance in vivo, nutritional labeling synthesis all by by serious
Impact.Performance the most intuitively is exactly that plant growing is slow, and stem and leaf becomes thin and weak, easily lodges, easily by insect pest so that normal plantation
Plant is unable to reach intended upgrowth situation.Agriculturally, potassium sulfate is main chlorideless potassic fertilizer, is also needed for crops are supplemented
The important sources of element sulphur.Because element sulphur can improve the yield of crops, and improve the quality of agricultural product, so potassium sulfate
Application in chemical fertilizer is particularly significant.
Current domestic process for producing potassium sulfate has two kinds:
One is potassium sulfate ore deposit or contains potassium salt through dissolving crystallized prepared potassium product, the potassium sulfate that this technique is produced
In product, impurity is high, crystallizes tiny, poorly water-soluble, it is impossible to meet the ingredient requirement of the water-soluble compound fertilizer of domestic production, more cannot be straight
Connect to fill as spray drop and use.
Potassium chloride is prepared potassium product through pyroreaction for Mannheim proeess by another kind, chloride ion content in this product
Height, product crystallization is tiny, poorly water-soluble.
The potassium sulfate that in prior art, two kinds of methods prepare all is difficult to meet agricultural modernization in sprinkling irrigation, drip irrigation
The requirement standard of chemical fertilizer application, needs the process preparing full water-soluble potassium sulfate badly, meets agricultural modernization plantation operation
Requirement.
Summary of the invention
It is an object of the invention to overcome in prior art, potassium sulfate prepared by process for producing potassium sulfate is difficult to full water
Molten characteristic, it is impossible to be applied to the problem in sprinkling irrigation, drip irrigation, it is provided that a kind of watersoluble potassium sulfate production technology.Prepared by the present invention
The most water-soluble potassium sulphate fertilizer there is good water soluble characteristic, it is possible to achieve without the effect of the residual of insoluble matter, for modernization
Agricultural production in the dissolving of feed liquid there is prominent effect.
In order to realize foregoing invention purpose, the invention provides techniques below scheme:
A kind of full water-soluble process for producing potassium sulfate, including following methods step:
(1) watersoluble potassium sulfate intermediate raw material one: use potassium sulfate ore deposit or the making from brine in potassium to obtain potassium sulfate.
Watersoluble potassium sulfate intermediate raw material two: use Mannheim proeess to prepare potassium sulfate.
(2) watersoluble potassium sulfate intermediate raw material one and watersoluble potassium sulfate intermediate raw material two being mixed, dissolve, extraction is filtered
Remove impurity, obtain potassium sulfate intermediate solution.
(3) by potassium sulfate intermediate solution crystallisation by cooling, watersoluble potassium sulfate is obtained.
The production technology of the full water-soluble potassium sulfate of the present invention, combines two kinds of different potassium sulfate raw materials in prior art
Preparation scheme, potassium sulfate production work of the prior art can be directly combined in the preparation process of full water-soluble potassium sulfate
Skill line, upgrading process is mild, and improvement cost is low, is conducive to improving the economic benefit of enterprise.
Meanwhile, potassium product prepared by the present invention belongs to the potassium product of full water-soluble, and belongs to complete water-soluble knot
Crystal potassium sulfate composition, purity is high.Sprinkling irrigation, application in drip irrigation when, the dissolution characteristics of chemical fertilizer is good, does not block shower nozzle/drip
Fill nozzle, significant for the agricultural production of modernization automatization.Owing to watersoluble potassium sulfate is the most water-soluble of crystal type
Potassium sulfate, it is also possible to be further applied to other field of fine chemical and use as raw material.Further, as compound fertilizer
Be mixed with raw material application, it may have greatly potentiality.
Compared with prior art, beneficial effects of the present invention:
1. the most domestic employing is obtained by the technique of the present invention with potassium sulfate ore deposit or the making from brine in potassium potassium sulfate and Mannheim proeess
The potassium sulfate prepared purifies through dissolving, abstraction impurity removal further, K in the crystal potassium sulfate produced2O >=52%, and product
Crystallize the thickest, be entirely dissolved in water.
2. the potassium sulfate that present invention process production prepares has the feature of very high purity, and corresponding product can not only be used for
Spray drip irrigation fertilizer directly uses, it is possible to as Water soluble fertilizer raw materials for production.
Accompanying drawing illustrates:
Fig. 1 is the process flow diagram of the present invention.
Detailed description of the invention
Below in conjunction with more specifically analytic explanation, explain some spy that technical scheme can have in the application
Property, it is simple to skilled artisan understands that technical scheme, propose the most simultaneously technical solution of the present invention part deformation/
Preferred embodiment.
The full water-soluble process for producing potassium sulfate of the present invention, in step (1), uses potassium sulfate ore deposit or the making from brine in potassium to obtain
The when of potassium sulfate intermediate raw material one, concrete preparation technology is as follows: if selecting potassium sulfate ore deposit, conventionally carry out sulfur
Watersoluble potassium sulfate intermediate raw material one is prepared in the processing of acid potassium；If selecting the salt in potassium, then will be as added sulphuric acid containing potassium salt
Salt, concentrates, and separates out crystal, obtains watersoluble potassium sulfate intermediate raw material one.
Further, concrete in step (1), when selecting potassium sulfate ore deposit when, by sulphuric acid potassium mine dissolution, dispersion, mistake
Filter, collects filtrate as watersoluble potassium sulfate intermediate raw material one.
Further, the described salt containing potassium refers to that liquid contains potassium resource, as bitter in bittern from salt-well brine, rich potassium salt lake bittern water or sea salt
Halogen, can be one of three of the above, it is also possible to be multiple mixed liquor.
Further, potassium content >=48% of described watersoluble potassium sulfate intermediate raw material one is (with K2O counts).In the middle of potassium sulfate
The source of raw material one is mainly based upon general potassium sulfate ore deposit or the salt in potassium prepares, and wherein the content of potassium element has
Limit, controls basic potassium content level more than 48%, had both ensured the disposable of raw material in the course of processing and can realize characteristic, and
Ensure that in the course of processing, the consumption of raw material controls within suitable level.
Further, described production technology, in step (1), use Mannheim proeess prepare potassium sulfate intermediate raw material two time
Waiting, the raw material of use is concentrated sulphuric acid and potassium chloride, wherein concentration >=98% of concentrated sulphuric acid, controls the mol ratio of sulphuric acid and potassium chloride
Example is 1.02-1.1:1.Ensure that the mole of concentrated sulphuric acid is the most excessive, promote carrying out and the conversion of reaction, improve the conversion of reaction
Rate, it is to avoid the chloride ion in reaction is mixed into potassium sulfate intermediate raw material two.Preferably, potassium sulfate intermediate raw material can prepared
It is added thereto to after two in carbonate and unnecessary sulphuric acid, hydrogen sulfate ion, obtains potassium sulfate sterling.
Further, potassium content >=50% of described watersoluble potassium sulfate intermediate raw material two is (with K2O counts).Mannheim legal system
Standby potassium sulfate intermediate raw material two has higher purity, during processed, controls the technological parameter of reaction, permissible
Preferably improve the purity of raw material, improve more preferable guarantee condition for preparing the potassium sulfate of full water-soluble.
Further, in described step (2), when extraction is filtered to remove impurity, the reagent A of addition extracts, this reagent
Most impurity component in removing potassium sulfate can be extracted, it is to avoid impurity component is blended in potassium sulfate solution, improve solution
Degree of purity, also promote follow-up crystallization, improve the quality grade of crystallization product.Described reagent A is (2-ethyl
Hexyl) phosphoric acid, any one or a few composition in (2-ethylhexyl) phosphonic acids list (2-ethylhexyl) fat and aphthenic acids mixed
Compound.Wherein, (2-ethylhexyl) phosphonic acids list (2-ethylhexyl) fat also writes 2-ethylhexyl phosphonic acid single 2-ethyl hexyl fat.
(2-ethylhexyl) phosphoric acid is also write: 2-ethylhexyl phosphoric acid.Containing below weight ratio in the most above-mentioned reagent A
One-tenth is grouped into: 1-3 part (2-ethylhexyl) phosphoric acid, 1-5 part (2-ethylhexyl) phosphonic acids list (2-ethylhexyl) fat and 1-3 part ring
Alkanoic acid.
Further, in described step (2), during filtration, use pressure filter to filter, high accuracy is preferably used and adds
Pressure pressure filter.Filter the high efficiency separation being capable of solid-liquid, reach to remove impurity component, not only include and be blended in potassium sulfate
Impurity, further comprises prepare in Process of Potassium Sulfate introduce interfering solid impurity.
Further, in described step (3), during crystallisation by cooling, add crystal seed, promote potassium sulfate crystallization.Described
Crystal seed is potassium sulfate crystal, the most miniature potassium sulfate crystalline particle, it is possible to the crystalline solid being effectively promoted potassium sulfate generates, and accelerates
The generation of potassium sulfate crystal, improves efficiency.
Further, described potassium ore deposit is alumstone ore.Typically rich in alunite composition in alumstone ore, mainly to contain
Potassium, sodium, aluminium sulfate mineral are the nonmetallic minerals of key component, typically process can prepare through simple floating method of washing
Potassium sulphate fertilizer, and association aluminum sulfate.
Further, in described full water-soluble potassium sulfate, water-insoluble≤0.05%, preferably water-insoluble≤0.03%.
Further, in described full water-soluble potassium sulfate, chlorine root≤0.1%, preferably chlorine root≤0.05%.
Further, in described full water-soluble potassium sulfate, moisture content≤3%, preferably moisture≤1%.
Further, in step (1), the concrete preparation method of watersoluble potassium sulfate intermediate raw material two can be preferably with lower section
Case: sulphuric acid and potassium chloride, is warmed up to 510-560 DEG C of reaction, preferably 520-550 DEG C reaction, preparation in the reacting furnace of Mannheim
Obtain potassium sulfate intermediate raw material two.Potassium content preferably wherein: K2O >=50%.
Further, in step (2), after potassium sulfate intermediate raw material one and potassium sulfate intermediate raw material two mixing, it is heated to 100-
120 DEG C, make material dissolution.Suitable heating up promotes the dissolving reaction of material, is conducive to adding the speed of fast response, improves and produce effect
Rate, it is also possible to making material mix more fully reliable, the quality of the slip obtained is more preferably.
Below in conjunction with test example and detailed description of the invention, the present invention is described in further detail.But this should not understood
Scope for the above-mentioned theme of the present invention is only limitted to below example, and all technology realized based on present invention belong to this
The scope of invention.
Embodiment 1
Complete water-soluble crystal process for producing potassium sulfate as described in Figure 1, obtains initially with potassium sulfate ore deposit or the making from brine in potassium
Potassium sulfate (K2O >=48%) and Mannheim proeess prepare potassium sulfate (K2O >=50%) it is raw material, through high-temperature digestion (100-120
DEG C), make complete water-soluble crystal potassium product after extraction filtering and impurity removing, more cooled crystallization.
Embodiment 2
Use the technique similar with embodiment 1, the potassium sulfate (K first obtained with potassium sulfate ore deposit or the making from brine in potassium2O≥
48%) being intermediate raw material one, the potassium ore deposit selected in the course of processing is alumstone ore；Then the sulphuric acid that Mannheim proeess prepares is used
Potassium, the concentrated sulphuric acid with 98% is as raw material, and the potassium chloride of 0.98 times of mole, is warmed up to 540 DEG C instead in the reacting furnace of Mannheim
Should, preparing potassium sulfate intermediate raw material two, purity is K2O >=50%.By the potassium sulfate intermediate raw material one and 100kg of 100kg
Potassium sulfate intermediate raw material two, mixing, be heated to 100-120 DEG C of high temperature in a kettle., make material the most fully dissolve.Then
Adding extractant to extract, the reagent A that extraction uses comprises the following ingredients: 2 parts of (2-ethylhexyl) phosphoric acid, 3 parts of (2-
Ethylhexyl) phosphonic acids list (2-ethylhexyl) fat and 2 parts of aphthenic acids formulated.After extraction filtering and impurity removing completes, then through cold
But complete water-soluble crystal potassium product is made after crystallization.
Other phosphate-containing ore can also be selected in potassium ore deposit in the present embodiment, it is generally preferable to uses the potassium ore deposit that potassium content is higher
Stone.
Embodiment 3
Use the technique similar with embodiment 1, the potassium sulfate (K first obtained with potassium sulfate ore deposit or the making from brine in potassium2O≥
48%) being intermediate raw material one, the potassium ore deposit selected in the course of processing is bittern from salt-well brine；Then, the sulphuric acid that Mannheim proeess prepares is used
Potassium, the concentrated sulphuric acid with 98% is as raw material, and the potassium chloride of 0.98 times of equivalent, is warmed up to 550 DEG C of reactions in the reacting furnace of Mannheim,
Preparing potassium sulfate intermediate raw material two, purity is K2O >=50%.Sulfur by the potassium sulfate intermediate raw material one and 100kg of 100kg
Acid potassium intermediate raw material two, mixing, it is heated to 100-120 DEG C of high temperature in a kettle., makes material the most fully dissolve.Add extraction
Agent extracts, and makes complete water-soluble crystal potassium product after extraction filtering and impurity removing, more cooled crystallization.
Bittern from salt-well brine belongs to common liquid and contains one of potassium resource, and the present embodiment uses the well salt hardship of commercial type
Halogen kind, the watersoluble potassium sulfate fertilizer preparation technology of certain present invention can also replace with rich potassium salt lake bittern water and bittern.
Test analysis 1
The watersoluble potassium sulfate product prepared for embodiment of the present invention 1-3 and two existing conventional sulfuric acid potassium produce
Product, commercially available watersoluble potassium sulfate fertilizer are analyzed, and result is as follows.
Table 1 potassium sulphate fertilizer product test analysis result
* commercially available watersoluble potassium sulfate is come from as the watersoluble potassium sulfate compared
From table 1, the watersoluble potassium sulfate product of the present invention not only potassium sulfate content is higher, hence it is evident that be better than general sulfur
Acid potassium fertilizer, and the pattern of product is preferable, and impurity component contained therein is few, and the residual quantity of chloride ion is the most extremely low, full
The sprinkling irrigation of foot agricultural modernization use, the chemical fertilizer Property requirements of drip irrigation, and it is more suitable for nothing owing to chloride ion content is extremely low
What chlorination was fertile is applied to not like the proportion of crop planting of chloride ion.
Test analysis 2
Watersoluble potassium sulfate product embodiment of the present invention 1-3 prepared and two existing conventional sulfuric acid potassium produce
Product, commercially available watersoluble potassium sulfate fertilizer are applied to drip irrigation farm, test for a long time (six months), the complete water-soluble sulfur of relative analysis
Whether acid potash fertilizer exists blockage problem for droping irrigating pipe, and result is as follows.
Table 2 farm test result
From the test result of table 2, the drip irrigation system of the full water-soluble potassium sulfate of the present invention is used preferably to protect
Hold long-time stability, it is to avoid unnecessary shower nozzle blocking, simultaneously in long term test, still further it can be seen that the complete water-soluble sulfur of the present invention
Acid potash fertilizer also has good inhibiting effect for the accumulation of the deposit of pipe interior, shows that the watersoluble potassium sulfate of the present invention is fertile
Be difficult to separate out deposit, for sprinkling irrigation, drip irrigation system pipeline there is good facilitation steadily in the long term.
Claims (10)
1. a full water-soluble process for producing potassium sulfate, including following methods step:
(1) watersoluble potassium sulfate intermediate raw material one: use potassium sulfate ore deposit or the making from brine in potassium to obtain potassium sulfate；
Watersoluble potassium sulfate intermediate raw material two: use Mannheim proeess to prepare potassium sulfate；
(2) watersoluble potassium sulfate intermediate raw material one and watersoluble potassium sulfate intermediate raw material two being mixed, dissolve, extraction is filtered to remove
Impurity, obtains potassium sulfate intermediate solution；
(3) by potassium sulfate intermediate solution crystallisation by cooling, watersoluble potassium sulfate is obtained.
2. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that in step (1), use potassium sulfate
The when that ore deposit or the making from brine in potassium obtaining potassium sulfate intermediate raw material one, concrete preparation technology is as follows:
If selecting potassium sulfate ore deposit, watersoluble potassium sulfate intermediate raw material one is prepared in the processing conventionally carrying out potassium sulfate；
If selecting the salt in potassium, then will concentrate as added sulfate containing potassium salt, separate out crystal, obtain watersoluble potassium sulfate
Intermediate raw material one.
3. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that in step (1), when selecting sulphuric acid
The when of potassium ore deposit, by sulphuric acid potassium mine dissolution, dispersion, filter, collect filtrate as watersoluble potassium sulfate intermediate raw material one.
4. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that the described salt containing potassium refers to liquid
Containing potassium resource.
5. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that watersoluble potassium sulfate intermediate raw material one
Potassium content >=48%.
6. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that watersoluble potassium sulfate intermediate raw material two
Potassium content >=50%.
7. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that in described step (2), extracted
When filtering decontamination, the reagent A of addition extracts；Described reagent A is (2-ethylhexyl) phosphoric acid, (2-ethylhexyl) phosphine
The mixture of any one or a few composition in single (2-ethylhexyl) fat of acid and aphthenic acids.
8. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that in step (2), use during filtration
It is that pressure filter filters.
9. full water-soluble process for producing potassium sulfate as claimed in claim 1, it is characterised in that in described step (3), cooling knot
Crystal seed is added during crystalline substance.
10. full water-soluble process for producing potassium sulfate as claimed in claim 9, it is characterised in that described crystal seed is that potassium sulfate is brilliant
Body.
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| 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 |
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| CN112158862B (en) * | 2020-05-15 | 2021-06-29 | 青岛碱业钾肥科技有限公司 | Production method of low-chlorine potassium sulfate |
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