CN107540415B - Method for preparing potash magnesium sulphate fertilizer by using potassium chloride and picromerite - Google Patents
Method for preparing potash magnesium sulphate fertilizer by using potassium chloride and picromerite Download PDFInfo
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- CN107540415B CN107540415B CN201710773737.0A CN201710773737A CN107540415B CN 107540415 B CN107540415 B CN 107540415B CN 201710773737 A CN201710773737 A CN 201710773737A CN 107540415 B CN107540415 B CN 107540415B
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- potassium chloride
- magnesium sulphate
- solid
- picromerite
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 110
- 239000003337 fertilizer Substances 0.000 title claims abstract description 76
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 72
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract description 66
- 229940072033 potash Drugs 0.000 title claims abstract description 66
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 title claims abstract description 66
- 235000015320 potassium carbonate Nutrition 0.000 title claims abstract description 66
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 55
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 55
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 36
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000012141 concentrate Substances 0.000 claims abstract description 41
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 24
- 238000005188 flotation Methods 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000013505 freshwater Substances 0.000 claims abstract description 11
- 239000012452 mother liquor Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- GMLLYEDWRJDBIT-UHFFFAOYSA-J magnesium;dipotassium;disulfate Chemical compound [Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GMLLYEDWRJDBIT-UHFFFAOYSA-J 0.000 claims 3
- 239000011777 magnesium Substances 0.000 abstract description 33
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 25
- 239000011591 potassium Substances 0.000 abstract description 25
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 23
- 229910052749 magnesium Inorganic materials 0.000 abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 13
- 239000011593 sulfur Substances 0.000 abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 abstract description 13
- 235000015097 nutrients Nutrition 0.000 abstract description 6
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229940091250 magnesium supplement Drugs 0.000 description 22
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 8
- 229910052939 potassium sulfate Inorganic materials 0.000 description 8
- 235000011151 potassium sulphates Nutrition 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical compound [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 description 6
- 235000021049 nutrient content Nutrition 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- HAQAPRXIBNGFQH-UHFFFAOYSA-N [V].[K].[Mg] Chemical compound [V].[K].[Mg] HAQAPRXIBNGFQH-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- SWHAQEYMVUEVNF-UHFFFAOYSA-N magnesium potassium Chemical compound [Mg].[K] SWHAQEYMVUEVNF-UHFFFAOYSA-N 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 244000061176 Nicotiana tabacum Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 244000309464 bull Species 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229960003390 magnesium sulfate Drugs 0.000 description 2
- 229940076230 magnesium sulfate monohydrate Drugs 0.000 description 2
- LFCFXZHKDRJMNS-UHFFFAOYSA-L magnesium;sulfate;hydrate Chemical compound O.[Mg+2].[O-]S([O-])(=O)=O LFCFXZHKDRJMNS-UHFFFAOYSA-L 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- GTXYBTOVMWVESR-UHFFFAOYSA-N [K].[Mg].[S] Chemical compound [K].[Mg].[S] GTXYBTOVMWVESR-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- -1 fruit trees Chemical compound 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical group [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Fertilizers (AREA)
Abstract
A method for preparing a potash magnesium sulphate fertilizer by using potassium chloride and picromerite comprises the following steps: (1) mixing the potassium chloride concentrate obtained by flotation with the picromerite concentrate obtained by flotation, adding fresh water, heating, stirring and mixing; (2) carrying out double decomposition reaction on the solid-liquid mixture slurry obtained in the step (1) in a constant temperature environment of 50-55 ℃ for 40-90 min to obtain a slurry after the reaction; (3) filtering the slurry obtained in the step (2) at constant temperature of 50-55 ℃ after reaction to realize solid-liquid separation, and obtaining solid S and mother liquor L; (4) and (4) drying the solid S obtained in the step (3) to obtain a potash magnesium sulphate fertilizer product. Product K of the invention2The content of O is high, the proportion of potassium, magnesium and sulfur nutrients is reasonable, the water solubility is good, the quality guarantee period is long, the production cost is low, the added value of the product is high, the process flow is simple, and the large-scale production is easy to realize.
Description
Technical Field
The invention relates to a preparation method of a high-quality potash magnesium sulphate fertilizer, in particular to a method for preparing the high-quality potash magnesium sulphate fertilizer by double decomposition reaction of potassium chloride and picromerite.
Background
Compared with the traditional potassium sulfate product, the potassium magnesium sulfate fertilizer increases magnesium medium elements, can promote the formation of chlorophyll, improve the yield and quality of crops, prolong the storage period of fruits, and is more suitable for being applied to economic crops such as vegetables, fruit trees, tobacco, tea leaves, flowers and the like.
At present, two common potash magnesium fertilizers on the market are providedOne is a domestic traditional potash magnesium sulphate fertilizer, which is extracted from salt lake brine or solid potash magnesium ore by a physical method and has water-soluble potassium content (K)2O)22 to 24 percent, water-soluble magnesium content of 5 to 11 percent and water-soluble sulfur content of 14 to 16 percent; the other is imported potash magnesium fertilizer, which is made by mixing potassium sulfate and picromerite after removing crystal water, and the water-soluble potassium content (K) of the fertilizer2O) is more than or equal to 40 percent, the content of water-soluble magnesium is more than or equal to 3 percent, and the content of water-soluble sulfur is more than or equal to 18 percent.
The domestic potash magnesium sulphate fertilizer mainly comprises soft potassium magnesium vanadium dehydration series products with the molecular formula of K2Mg(SO4)2·nH2O (n = 4-6), the execution standard is GB/T20937-2007, and the high-grade product requirement is water-soluble potassium (K)2O) is more than or equal to 30 percent, water-soluble magnesium (Mg) is more than or equal to 7 percent, and water-soluble sulfur (S) is more than or equal to 18 percent; first-class requirement is water-soluble potassium (K)2O) is more than or equal to 24 percent, water-soluble magnesium (Mg) is more than or equal to 6 percent, and water-soluble sulfur (S) is more than or equal to 16 percent; the qualified product is water-soluble potassium (K)2O) is more than or equal to 21 percent, water-soluble magnesium (Mg) is more than or equal to 5 percent, and water-soluble sulfur (S) is more than or equal to 14 percent. Due to picromerite K2The content of 0 is low, the potassium, magnesium and sulfur nutrients are not reasonably matched, and the growth effect of various chlorine-avoiding crops is not obvious. Meanwhile, the potash magnesium sulphate fertilizer contains more crystal water, is easy to cake in the south with humid and sultry climate, is easy to deliquesce after being unpacked, and has a shelf life of less than seven days under non-sealed packing, so that the domestic potash magnesium sulphate fertilizer has lower market acceptance, limited sales and low market price in the potash fertilizer market.
At present, the production method of potassium magnesium sulfate fertilizer in China mainly adopts the processes of conversion, flotation, washing and drying, namely KCl and MgSO in potassium mixed salt raw ore are added with water4·7H2And converting the O into soft potassium magnesium vanadium, enriching the soft potassium magnesium vanadium by adopting a flotation process, and washing and drying the concentrate to obtain a qualified potash magnesium sulphate fertilizer product. The processing cost of the potash magnesium sulphate fertilizer product of the process has certain difference due to the grade of the raw ore, and is generally 900-1000 yuan/ton. When market conditions of potash magnesium sulphate fertilizer products are good, several potash fertilizer production enterprises in Xinjiang and Qinghai produce the traditional potash magnesium sulphate fertilizer products. However, as the market of potash fertilizers is continuously low, the price of the traditional potash magnesium sulphate fertilizer is only 1100-1200 yuan/ton, and the production enterprises bringThe production enthusiasm of enterprises is not high due to serious loss, production is stopped at present, and the potassium sulfate is produced after the process is transformed.
Compared with domestic potash magnesium sulphate fertilizer which is sold late and low in price, the imported high-quality potash magnesium sulphate fertilizer is very pretty, the current market price is up to 4600 yuan/ton, the quality guarantee period is relatively long under non-sealed package, the potash magnesium sulphate fertilizer is widely popular in the potash fertilizer market, and the user evaluation is high. The imported potassium magnesium sulfate fertilizer is mainly 'red bull' potassium magnesium sulfate developed by German potassium salt group. The difference between the effective nutrient of the potash magnesium sulphate fertilizer and the domestic potash magnesium sulphate fertilizer is mainly reflected in K2The content of O. The product contains water soluble potassium (K)2O) is more than or equal to 40 percent, water-soluble magnesium (Mg) is more than or equal to 3 percent, water-soluble sulfur (S) is more than or equal to 18 percent, the main component is a mixture of potassium sulfate and magnesium sulfate monohydrate, and the processing technology mainly adopts the mixing of the potassium sulfate produced in a salt pan and the magnesium sulfate monohydrate according to a certain proportion, so the processing cost of the product is about 1500-1600 yuan/ton. Due to its K2High content of O and medium element Mg2+、SO4 2-The nutrient matching proportion is reasonable, and the fertilizer is very suitable for the growth of various crops which are forbidden to eat chlorine, such as fruit trees, melons, tobacco, tea leaves and the like, so that the market price of the fertilizer exceeds the price of potassium sulfate. However, the imported red bull potassium magnesium sulfate product also has the defects of high content of water-insoluble substances (the content of the water-insoluble substances is more than 4.8 percent), higher price, inapplicability to drip irrigation fertilization and the like.
Chinese patent application CN 102320867A (potash magnesium sulphate fertilizer and manufacturing method thereof) mainly aims at the improvement of granulation equipment and process parameters of potash magnesium fertilizer products, and the water-soluble potassium (K) of the potash magnesium fertilizer products2O) content of 22-26 percent, belonging to the domestic traditional potash magnesium fertilizer. Chinese patent application CN 102515881A (process for preparing potash magnesium sulphate fertilizer by using mud-containing potassium mixed salt ore) mainly aims at obtaining traditional potash magnesium sulphate fertilizer product by adopting ore washing desliming-flotation-washing process aiming at primary mud-containing potassium mixed salt ore, and water-soluble potassium (K) of the product2O) content reaches 24 percent. Chinese patent application CN 102850124 a (potash magnesium sulphate fertilizer and its preparation method) discloses a method for preparing new potash magnesium sulphate fertilizer by adding trace element compound into traditional potash magnesium fertilizer, which has the characteristics of high solubility, high strength, etc., but its water-soluble potassium (K) is2O) content of only 25.98% of the total weight of the composition. Chinese patent application CN 103172451A (a new potash magnesium sulphate fertilizer and its preparation method) mainly introduces a method for preparing a new potash magnesium sulphate fertilizer by blending trace elements such as manganese, zinc, boron, etc. with potassium sulfate and magnesium sulfate, the new potash magnesium sulphate fertilizer has the advantages of fast fertilizer effect, comprehensive nutrition, simple application, etc., but its water-soluble potassium (K) is2O) content is only 22%. Chinese patent application CN 103936523A (a production method of slow-release potassium magnesium fertilizer) mainly introduces a process for preparing slow-release potassium magnesium fertilizer by using potassium chloride or potassium sulfate to react with magnesium chloride or magnesium sulfate and ammonium bicarbonate, wherein the slow-release potassium magnesium fertilizer mainly contains KHCO3·MgCO3·4H2O, S, water-soluble potassium (K) without nutrient2O) content 18.36%. Chinese patent application CN 104261940A (a preparation method of potash magnesium fertilizer) discloses a process for preparing potash magnesium sulphate fertilizer by conversion and flotation by using high magnesium salt lake brine, mirabilite and potassium chloride and phase diagram theoretical knowledge, which has the advantages of low energy consumption, low cost, simple process flow, short production period and the like, but the water-soluble potassium (K) is water-soluble2O) content is only about 22 percent. Chinese patent application CN 104311164A (a production method of potash magnesium sulphate fertilizer) discloses a method for preparing potash magnesium sulphate fertilizer by using potassium chloride, concentrated sulfuric acid and magnesium oxide as raw materials, and the obtained potash magnesium sulphate fertilizer is still the traditional potash magnesium sulphate fertilizer and has water-soluble potassium (K)2O) content is only 24% (GB/T20937-2007 first-grade potassium magnesium sulfate fertilizer).
Water-soluble potassium (K) in potash magnesium fertilizer obtained in the above-mentioned published patent documents2O) content is less than 26 percent, water insoluble substance content is generally more than 3.0 percent, market price is generally 1100 yuan/ton-1200 yuan/ton, and the water soluble potassium (K) is 40 percent of the novel foreign high-quality potash magnesium sulphate fertilizer2O) content and 4600 yuan/ton, has large difference in market price, low acceptance of wide users and poor market reaction, and is not widely applied to crop planting.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a method for preparing a potash magnesium sulphate fertilizer by using potassium chloride and picromerite, and the obtained high-quality potash magnesium sulphate fertilizer product K2High O content, reasonable ratio of potassium, magnesium and sulfur nutrients, good water solubility, long shelf life, low production cost and high added value of products.
The technical scheme adopted by the invention for solving the technical problem is that,
a method for preparing a potash magnesium sulphate fertilizer by using potassium chloride and picromerite comprises the following steps:
(1) mixing the potassium chloride concentrate obtained by flotation with the picromerite concentrate obtained by flotation, adding fresh water, heating, stirring and mixing;
in the invention, the fresh water is water with the salt content less than or equal to 5 wt%.
(2) Carrying out double decomposition reaction on the solid-liquid mixture slurry obtained in the step (1) in a constant temperature environment of 50-55 ℃ for 40-90 min to obtain a slurry after the reaction;
(3) filtering the slurry obtained in the step (2) at constant temperature of 50-55 ℃ after reaction to realize solid-liquid separation, and obtaining solid S and mother liquor L;
(4) and (4) drying the solid S obtained in the step (3) to obtain a high-quality potash magnesium sulphate fertilizer product.
Further, in the step (1), the quality composition of the potassium chloride concentrate ions obtained by flotation comprises K+26.45%～51.56%、Mg2+0.30%～2.76%、Na+0.73%～7.35%、Cl-37.51%～48.39%、SO4 2-0.50 to 7.93 percent. The ionic mass composition of the picromerite concentrate obtained by flotation comprises K+14.84%～16.58%、Mg2+5.31%～6.01%、Na+0.94%～3.59%、Cl-5.00%～7.60%、SO4 2-36.40-39.30 percent. The mass ratio of the potassium chloride concentrate obtained by flotation to the soft leonite concentrate obtained by flotation is (ratio) potassium chloride concentrate to soft leonite concentrate = 0.40-0.63: 1. The adding amount of the fresh water is 54.54 to 67.00 percent of the sum of the quality of the potassium chloride concentrate and the picromerite concentrate. The heating, stirring and mixing temperature is 50-55 ℃.
Further, in the step (3), the solid S is a wet base material, and the ion mass composition of the solid S comprises K+27.81%～33.92%、Mg2+2.98%～4.45%、Na+0.50%～0.66%、Cl-0.25%～0.50%、SO4 2-52.10% -54.32%; the ionic mass composition of the mother liquor L comprises K+7.39%～8.31%、Mg2+2.41%～2.57%、Na+0.50%～0.56%、Cl-9.81%～11.20%、SO4 2-5.73%～7.07%。
Further, in the step (4), the drying temperature of the solid S is 250-280 ℃.
The potash magnesium sulphate fertilizer product obtained by the invention has effective nutrient content of water-soluble potassium (K)2O mass) is more than or equal to 35 percent, water-soluble magnesium (based on the mass of Mg) is more than or equal to 3 percent, and water-soluble sulfur (based on the mass of S) is more than or equal to 17 percent.
K is the potash magnesium sulphate fertilizer product obtained by the invention2The method has the advantages of high O content, reasonable potassium-magnesium-sulfur nutrient proportion, good water solubility (the content of water-insoluble substances is less than 2.0wt%), long shelf life (more than one month) under non-sealed package, simple process flow, easy realization of large-scale production, relatively low production cost of products and high added value.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The embodiment comprises the following steps:
(1) the mass composition comprises K+26.45%、Mg2+2.76%、Na+7.35%、Cl-37.51%、SO4 2-7.93% of the potassium chloride concentrate obtained by flotation and having a mass composition comprising K+14.84%、Mg2+5.31%、Na+3.59%、Cl-7.60%、SO4 2-36.40% of the picromerite concentrate obtained by flotation is added into a reaction vessel according to the mass ratio of the potassium chloride concentrate to the picromerite concentrate =0.40 to 1, and then fresh water with the mass of 54.54% of the sum of the potassium chloride concentrate and the picromerite concentrate is added; heating to 50 deg.C and stirring;
in the invention, the fresh water is water with the salt content less than or equal to 5 wt%.
(2) Stirring and reacting the solid-liquid mixture slurry obtained in the step (1) for 40min in a constant temperature environment at the temperature of 50 ℃ to obtain reacted slurry;
(3) filtering the slurry obtained in the step (2) after reaction at a constant temperature of 50 ℃ for solid-liquid separation to obtain reacted solid S and reacted mother liquor L;
(4) the solid S obtained in the step (3) is a wet-based material, and the ion mass composition of the solid S comprises K+27.81%、Mg2+4.45%、Na+0.50%、Cl-0.50%、SO4 2-52.10 percent. The ionic mass composition of the mother liquor L comprises K+7.39%、Mg2+2.57%、Na+0.55%、Cl-9.81%、SO4 2-7.07 percent. Drying and dehydrating the solid S at 250 ℃ to obtain a potash magnesium sulphate fertilizer product with the effective nutrient content of water-soluble potassium (K)2O mass) 35.26%, water-soluble magnesium (Mg by mass of Mg)4.68%, water-soluble sulfur (by mass of S) 17.37%.
The high-quality potash magnesium sulphate fertilizer has high dissolution speed, the content of water insoluble substances is less than 2.0wt%, the quality guarantee period can reach more than 1 month under the condition of non-sealed package in high-temperature and humid regions (such as 8 months of Changsha in Hunan), the production cost of the product is 1200 yuan/ton, and the delivery sale price can reach 3000 yuan/ton.
Example 2
The embodiment comprises the following steps:
(1) ion mass composition including K+28.86%、Mg2+2.49%、Na+6.13%、Cl-39.06%、SO4 2-5.19% potassium chloride flotation concentrate and ion mass composition including K+15.13%、Mg2+5.83%、Na+2.91%、Cl-7.11%、SO4 2-38.05% of picromerite flotation concentrate is added into the reaction vessel according to the mass ratio of potassium chloride concentrate to picromerite concentrate =0.63 to 1, and fresh water with the mass of 67.00% of the sum of the mass of potassium chloride concentrate and picromerite concentrate is added. The temperature for heating, stirring and mixing was 53 ℃.
(2) Carrying out double decomposition reaction on the solid-liquid mixture slurry obtained in the step (1) for 50min in a constant temperature environment at 53 ℃ to obtain a slurry after the reaction;
(3) the slurry obtained in the step (2) after reaction is at 53 DEG CFiltering at constant temperature for solid-liquid separation to obtain reacted solid S and reacted mother liquor L; the solid S is a wet base material and the ionic mass composition of the solid S comprises K+29.36%、Mg2+4.03%、Na+0.66%、Cl-0.32%、SO4 2-52.91%, the ionic mass composition of the mother liquor L includes K+8.27%、Mg2+2.41%、Na+0.56%、Cl-11.05%、SO4 2-5.89%。
(4) And (4) drying and dehydrating the solid S obtained in the step (3) at 270 ℃ to obtain a potash magnesium sulphate fertilizer product. The effective nutrient content is water soluble potassium (expressed as K)2O mass) 37.23%, water-soluble magnesium (in terms of Mg mass) 4.24%, water-soluble sulfur (in terms of S mass) 17.64%.
The high-quality potash magnesium sulphate fertilizer has high dissolution speed, the content of water insoluble substances is less than 2.0wt%, the quality guarantee period can reach 1 month under non-sealed package in high-temperature and humid areas (such as 8 months of Changsha in Hunan), the production cost of the product is 1100 yuan/ton, and the factory sale price can reach 3000 yuan/ton.
Example 3
The embodiment comprises the following steps:
(1) ion mass composition including K+51.56%、Mg2+0.30%、Na+0.73%、Cl-48.39%、SO4 2-0.50 percent of potassium chloride flotation concentrate and ions comprise the following components of K+16.58%、Mg2+6.01%、Na+0.94%、Cl-5.00%、SO4 2-39.30% of picromerite flotation concentrate is added into a reaction vessel according to the mass ratio of potassium chloride concentrate to picromerite concentrate =0.47 to 1, and then fresh water with the mass being 58.79% of the sum of the mass of potassium chloride concentrate and picromerite concentrate is added; heating at 55 deg.C, stirring, and mixing;
(2) carrying out double decomposition reaction on the solid-liquid mixture slurry obtained in the step (1) for 60min in a constant temperature environment of 55 ℃ to obtain a slurry after the reaction;
(3) filtering the slurry obtained in the step (2) at the constant temperature of 55 ℃ for solid-liquid separation to obtain reacted solid S and reacted mother liquor L; the solid S is a wet base material and the ionic mass composition of the solid S comprises K+33.92%、Mg2+2.98%、Na+0.59%、Cl-0.25%、SO4 2-54.32 percent; the ionic mass composition of the mother liquor L comprises K+8.31%、Mg2+2.44%、Na+0.50%、Cl-11.20%、SO4 2-5.73%。
(4) Drying and dehydrating the solid S obtained in the step (3) at 280 ℃ to obtain a potash magnesium sulphate fertilizer product with effective nutrient content of water-soluble potassium (K)2O mass) 43.01%, water-soluble magnesium (in terms of Mg mass) 3.14%, water-soluble sulfur (in terms of S mass) 18.11%.
The high-quality potash magnesium sulphate fertilizer has high dissolution speed, the content of water insoluble substances is less than 2.0wt%, the quality guarantee period can reach 1 month under non-sealed package in high-temperature and humid areas (such as 8 months of Changsha in Hunan), the production cost of the product is 1000 yuan/ton, and the factory sale price can reach 3000 yuan/ton.
Claims (6)
1. A method for preparing a potash magnesium sulphate fertilizer by using potassium chloride and picromerite is characterized by comprising the following steps:
(1) mixing the potassium chloride concentrate obtained by flotation with the picromerite concentrate obtained by flotation, adding fresh water, heating, stirring and mixing; the quality composition of potassium chloride concentrate ions obtained by flotation comprises K+26.45%～51.56%、Mg2+0.30%～2.76%、Na+0.73%～7.35%、Cl-37.51%～48.39%、SO4 2-0.50% -7.93%; the ionic mass composition of the picromerite concentrate obtained by flotation comprises K+14.84%～16.58%、Mg2+5.31%～6.01%、Na+0.94%～3.59%、Cl-5.00%～7.60%、SO4 2-36.40% -39.30%; the mass ratio of the potassium chloride concentrate obtained by flotation to the soft leonite concentrate obtained by flotation is that the ratio of the potassium chloride concentrate to the soft leonite concentrate is = 0.40-0.63: 1;
the fresh water is water with the salt content of less than or equal to 5 wt%;
(2) carrying out double decomposition reaction on the solid-liquid mixture slurry obtained in the step (1) in a constant temperature environment of 50-55 ℃ for 40-90 min to obtain a slurry after the reaction;
(3) filtering the slurry obtained in the step (2) at constant temperature of 50-55 ℃ after reaction to realize solid-liquid separation, and obtaining solid S and mother liquor L;
(4) and (4) drying the solid S obtained in the step (3) to obtain a potash magnesium sulphate fertilizer product.
2. The method for preparing the potash magnesium sulphate fertilizer by utilizing potassium chloride and schoenite, as claimed in claim 1, wherein in the step (1), the amount of fresh water added is 54.54% -67.00% of the sum of the mass of the potassium chloride concentrate and the schoenite concentrate.
3. The method for preparing the potash magnesium sulphate fertilizer by using potassium chloride and picromerite as claimed in claim 1 or 2, wherein the temperature for heating, stirring and mixing in the step (1) is 50-55 ℃.
4. The process for preparing potash magnesium sulphate fertilizer using potassium chloride and picromerite as claimed in claim 1 or 2, wherein in step (3), the solid S is a wet base material with an ionic mass composition comprising K+27.81%～33.92%、Mg2+2.98%～4.45%、Na+0.50%～0.66%、Cl-0.25%～0.50%、SO4 2-52.10%～54.32%。
5. The method for preparing potash magnesium sulphate fertilizer using potassium chloride and picromerite as claimed in claim 1 or 2, wherein in step (3), the ion mass composition of mother liquor L comprises K+7.39%～8.31%、Mg2+2.41%～2.57%、Na+0.50%～0.56%、Cl-9.81%～11.20%、SO4 2-5.73%～7.07%。
6. The method for preparing the potash magnesium sulphate fertilizer by using potassium chloride and schoenite as claimed in claim 1 or 2, wherein the drying temperature of the solid S in the step (4) is 250-280 ℃.
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| CN115872786A (en) * | 2022-10-26 | 2023-03-31 | 国投新疆罗布泊钾盐有限责任公司 | Method for producing various potash magnesium sulphate fertilizer products according to different nutrient requirements |
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