CN104311164A - Production method of potash magnesium sulfate fertilizer - Google Patents

Production method of potash magnesium sulfate fertilizer Download PDF

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Publication number
CN104311164A
CN104311164A CN201410526143.6A CN201410526143A CN104311164A CN 104311164 A CN104311164 A CN 104311164A CN 201410526143 A CN201410526143 A CN 201410526143A CN 104311164 A CN104311164 A CN 104311164A
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China
Prior art keywords
slip
magnesium sulfate
potash
potassium
magnesium oxide
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CN201410526143.6A
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Chinese (zh)
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李彬
张洪江
杨柳
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LOMON LAND AGRICULTURE Co Ltd
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LOMON LAND AGRICULTURE Co Ltd
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    • 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
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D5/00—Fertilisers containing magnesium

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

The invention discloses a production method of a potash magnesium sulfate fertilizer. According to the production method, potassium chloride, concentrated sulfuric acid and magnesium oxide are taken as raw materials; the potassium chloride reacts with the concentrated sulfuric acid to obtain potassium hydrogen sulfate slurry; the potassium hydrogen sulfate slurry reacts with a magnesium oxide slurry to obtain potash magnesium sulfate slurry, and finally, the potash magnesium sulfate slurry is cooled, crushed and dried to obtain the potash magnesium sulfate fertilizer. The preparation method of the potash magnesium sulfate fertilizer is wide in raw material source, high in product yield and low in production cost. A potassium chloride low-temperature transformation production process is adopted, the raw materials are added according to a formula in batches, the process flow is simple and easy to control, and the quality of the product can be completely guaranteed; and the grade of the obtained potash magnesium sulfate fertilizer is up to or exceeds the national potash magnesium sulfate fertilizer first-grade standard.

Description

A kind of production method of potash magnesium sulphate fertilizer
Technical field
The present invention is specifically related to a kind of production method of potash magnesium sulphate fertilizer, belongs to technical field of chemical fertilizer production.
Background technology
The molecular formula of potash magnesium sulphate fertilizer is K 2sO 4m (MgSO 4) nH 2o(is m=1 ~ 2 wherein, n=0 ~ 6), it is a kind of inorganic green fertilizer being rich in K, Mg, S tri-kinds of nutrients, water-soluble fabulous, potassium, magnesium and element sulphur can not only be provided to plant and energy chessom, promote growing of the leaf of plant, branch and root system, make root system of plant huge, plant can be impelled simultaneously to accelerate to absorb the element such as Nitrogen In Soils, phosphorus, increase the ability of plant resistant disease.Potassium magnesium sulfate belongs to chemically neutral salt, and use and can not affect P in soil H value, chloride content is low in addition, and the Effects of Salinity of long-term application to soil is less.
At the annual amount of application of U.S.'s potash magnesium sulphate fertilizer at hundreds of thousands of ton, also a large amount of for preparing composite fertilizer except directly using, according to soil quality and the crop situation preparation special fertilizer on each farm.New variety of potash fertilizer series are still belonged at Chinese potash magnesium sulphate fertilizer.At present, potash magnesium sulphate fertilizer is worldwide widely used, and 30% of U.S.'s potash magnesium sulphate fertilizer brand " Shi Baomi " ultimate production sells to Mexico, Costa Rica, Colombia, Brazil, Venezuela, Ecuador, Peru, Australia, Japan, Korea S, Philippines, Malaysia, Thailand and some areas, Europe etc.Typically " Shi Baomi " chemical constitution is: w (K 2o)=22%, w (Mg)=11% and w (S)=22%, its most important proterties is solubility good (100% is water-soluble), but solubleness is slightly lower than Repone K.Another important character of " Shi Baomi " is that its composition is mainly neutral salt, uses and can not affect P in soil H.Because its composition is mainly sulfate radical, chlorine ions mark is lower than 1.5%, and thus its salt index is relatively low.Compared with traditional potassium product, potash magnesium sulphate fertilizer adds magnesium moderate-element, for crop provides nutrient balanced more comprehensively.Along with China's soil salinization problem is increasingly severe, replace the status of Repone K in agricultural planting gradually without chlorine high-quality potash fertilizer (potassium sulfate and potassium magnesium sulfate).
The raw material producing potash magnesium sulphate fertilizer in China is Shoenite ore deposit, and molecular formula is K 2mg (SO 4) 26H 2o is one of essential mineral of soluble potassium salt mine.The production method of potash magnesium sulphate fertilizer is divided into natural extract method and blending method two kinds according to raw material is different with technique.Natural extract method comprises and adopts salt lake brine or solid kalium-magnesium deposit through physical method direct production and adopt potassium magnesium navajoite direct production two kinds of techniques, shortcoming is larger by raw material supply limitations affect, technical process is comparatively complicated, operation controls inconvenient, and in the operating process of flotation and crystallization, accuracy requirement is higher.And blending method produces with potassium sulfate or Repone K and the simple blending of magnesium salts, the potash magnesium sulphate fertilizer that the method is produced is only the mixture of sulphate of potash and magesium, quality product is uneven, and it with the potassium sulfate of high price for raw material, cost advantage is obviously not enough.And whether the potash magnesium sulphate fertilizer adopting the simple blending mode such as potassium sulfate and magnesium oxide to produce can deserve to be called potash magnesium sulphate fertilizer, and mainly should see its chloride ion content, potassium content should be greater than Mg content simultaneously.But the potassium magnesium sulfate fertilizer product of some blending of selling in the market, although all contain potassium, sulphur, magnesium, some chlorion exceeds standard, and the Mg content of some product is greater than potassium content, and these products all do not reach the specification of quality of potash magnesium sulphate fertilizer.
Summary of the invention
Object of the present invention is just, for above-mentioned the deficiencies in the prior art, to provide the production method that a kind of potash magnesium sulphate fertilizer is new, and the method production technique is simple, and raw material sources are extensive, and cheap, production cost is low.
To achieve these goals, the technical solution used in the present invention is such:
A kind of production method of potash magnesium sulphate fertilizer, it is characterized in that: it with Repone K, the vitriol oil and magnesium oxide for raw material, Repone K and strong sulfuric acid response obtain sal enixum slip, sal enixum slip obtains potassium magnesium sulfate slip with magnesium oxide slip again, and namely potassium magnesium sulfate slip obtains potash magnesium sulphate fertilizer through cooling, fragmentation, baking operation.
Further, the preparation method of above-mentioned potassium magnesium sulfate slip comprises the following steps:
(1) prepare sal enixum slip: potassium chloride and vitriol oil mix and blend react 30-60min, hydrogen chloride gas is overflowed to obtain sal enixum slip, and wherein control temperature of reaction 80 ~ 140 DEG C, the mol ratio of Repone K and the vitriol oil is with KCl and H 2sO 4count 1:1 ~ 1.2;
(2) magnesium oxide slip is prepared: according to quality than magnesium oxide: water=1:0.5 ~ 2, magnesium oxide is mixed obtained magnesium oxide slip with water;
(3) potassium magnesium sulfate slip is prepared: the sal enixum slip obtained by step (1) and the magnesium oxide slip Hybrid Heating of step (2) are reacted 5 ~ 10min and namely obtained potassium magnesium sulfate slip, wherein controlling temperature of reaction is 120 ~ 160 DEG C, and the mol ratio of sal enixum slip and magnesium oxide slip is with KHSO 41:1 is got with MgO meter.
Further, in order to promote the reaction of sal enixum, described in step (1), Repone K mixes with the vitriol oil in the form of a solution, wherein concentration >=50% of Klorvess Liquid.
Equally, in order to sal enixum is produced in accelerated reaction, concentration >=90% of the vitriol oil described in step (1).
Further, the hydrogen chloride gas grading absorption that described step (1) is overflowed makes hydrochloric acid.
Compared with prior art, the invention has the advantages that: the present invention is with cheap Repone K, the vitriol oil and magnesium oxide for raw material, and principal reaction equation is:
KCl+H 2SO 4=KHSO 4+HCl↑
KHSO 4+MgO+(n-1)H 2O=K 2SO 4·MgSO 4·nH 2O?（1≤n≤6）
First by Repone K and vitriol oil hybrid reaction, by controlling temperature of reaction at 80 ~ 140 DEG C, obtain sal enixum slip, and hydrogen chloride gas is discharged in gaseous form under the condition of heating, react completely to ensure simultaneously, not chloride ion-containing in the sal enixum slip generated, the mol ratio of Repone K and the vitriol oil is with KCl and H 2sO 4count 1:1 ~ 1.2; The hydrogen chloride gas sectional of effusion absorbs makes hydrochloric acid to reach the recycling of waste gas.
Then magnesium oxide is mixed obtained magnesium oxide slip with water, with to make in its and sal enixum slip and time be convenient to stir, react completely, by control temperature of reaction 140 ~ 160 DEG C, the mol ratio of sal enixum slip and magnesium oxide slip is with KHSO 4get 1:1 with MgO meter, in magnesium oxide slip and sal enixum slip and completely, obtain potassium magnesium sulfate slip, this potassium magnesium sulfate slip obtains potassium magnesium sulfate fertilizer product through cooling, broken, oven dry.
The reaction of Repone K and sulfuric acid is replacement(metathesis)reaction, needs to control range of reaction temperature at 80 ~ 140 DEG C, and guarantee reaction generates purity sal enixum slip up to standard.If temperature is lower than 80 DEG C, it is clean that the hydrogenchloride that reaction generates is difficult to effusion, causes residual chloride hydrogen in sal enixum slip too much, make potassium magnesium sulfate fertilizer product chloride ion content not reach national standard requirement.If temperature is higher than 140 DEG C, the evaporation of reaction process moisture is too fast, needs constantly to supplement clear water to reaction vessel, causes sal enixum slip mobility variations large, be unfavorable for the control to reaction process, and the unit consumption of energy that control temperature crosses high product will increase considerably.The speed of reaction of Repone K and sulfuric acid is moderate, and the reaction times controls at 30-60min, can ensure to react completely.
Sal enixum and magnesian reaction are neutralization reaction, and temperature range controls at 120 ~ 160 DEG C, ensure that neutralization obtains potassium magnesium sulfate slip.If temperature is lower than 120 DEG C, rapid crystallization solidifies by the potassium magnesium sulfate slip that reaction generates, and affects residual sulfuric acid hydrogen potassium and magnesian continuation reaction.If temperature is higher than 160 DEG C, the evaporation of reaction process water is too fast, and potassium magnesium sulfate slip mobility will significantly reduce, and will affect sal enixum and magnesian abundant reaction equally.When temperature is lower than 120 DEG C or higher than 160 DEG C, all may make sal enixum and magnesium oxide can not complete reaction, cause content of magnesia in product too high, make product water insolubles content not reach national standard requirement.In addition, for ensureing that magnesium oxide and sal enixum can fully react, magnesium oxide should in advance according to quality than magnesium oxide: water=1:0.5 ~ 2 are mixed with slip, and the water yield added just in time can meet the needs of potassium magnesium sulfate crystal water and maintenance product adequate liquidity.If magnesium oxide: water ﹤ 1:2, the potassium magnesium sulfate slip mobility extreme difference of generation, is unfavorable for fully carrying out of reaction, insoluble content of magnesia in product is exceeded standard.If magnesium oxide: water ﹥ 1:0.5, the potassium magnesium sulfate water content that reaction is produced is too high, can not be directly broken after naturally cooling, and will increase the oven dry cost of product.Sal enixum and magnesian speed of reaction high, the reaction times controls at 5-10min, can ensure to react completely.
The preparation method of potash magnesium sulphate fertilizer provided by the present invention, with Repone K, magnesium oxide and sulfuric acid for raw material, Commercial sources is extensive, and product yield can reach 99%, and production cost is lower.
The present invention adopts potassium chloride low-temperature conversion method production technique, raw material adopts and adds by formula in batches, technical process is briefly easily controlled, and can ensure the quality of product completely, and the potash magnesium sulphate fertilizer obtained taste can meet or exceed national potash magnesium sulphate fertilizer acceptable end product standard (GB/20937-2007).
Embodiment
In order to the object of the present invention of understanding clearly, technical scheme and beneficial effect, below the present invention is described further, but not by protection scope of the present invention limit in the examples below.
Potash magnesium sulphate fertilizer product standard GB/T20937-2007 is applicable to only through the potassium magnesium sulfate fertilizer product containing the moderate-element such as magnesium, sulphur that physical method extracts or direct removing impurity is made from salt lake brine or solid kalium-magnesium deposit, and its standard content is as shown in the table:
Embodiment 1:
(1) sal enixum slip is prepared:
The 108.9Kg vitriol oil (H is added in reactor 2sO 4mass content 90%), stir and reacting by heating still to 80 DEG C, then in reactor, add 149Kg Klorvess Liquid (KCl mass content 50%), keep reactor temperature to be 80 DEG C of Keep agitation 30min, hydrogen chloride gas is all overflowed, obtains sal enixum slip 221.4Kg(KHSO 4mass content 61.4%).
(2) magnesium oxide slip is prepared:
In plastic tank, add 40Kg magnesium oxide and 20Kg clear water, stir preparation and obtain magnesium oxide slip 60Kg (MgO mass content 66.7%) for subsequent use.
(3) neutralization reaction:
The magnesium oxide slip of (2) being joined joins in the sal enixum slip of (1) gained, reacting by heating still temperature to 120 DEG C, and Keep agitation reaction 5 ~ 10min obtains potassium magnesium sulfate slip.
(4) crushing drying is cooled:
Opening reactor discharge valve is put in stock pan by molten for the potassium magnesium sulfate of generation slurry, and be crushed to below 1mm after naturally cooling solidifies, oven drying at low temperature obtains potassium magnesium sulfate fertilizer product.
Embodiment 2:
(1) sal enixum slip is prepared:
The 105.4Kg vitriol oil (H is added in reactor 2sO 4mass content 93%), stir and reacting by heating still to 120 DEG C, then in reactor, add 120.2Kg Klorvess Liquid (KCl mass content 62%), keep reactor temperature to be 120 DEG C of Keep agitation 45min, hydrogen chloride gas is all overflowed, obtains sal enixum slip 189.1Kg(KHSO 4mass content 71.9%).
(2) magnesium oxide slip is prepared:
In plastic tank, add 40Kg magnesium oxide and 40Kg clear water, stir preparation and obtain magnesium oxide slip 80Kg (MgO mass content 50%) for subsequent use.
(3) neutralization reaction:
The magnesium oxide slip of (2) being joined joins in the sal enixum slip of (1) gained, reacting by heating still temperature to 140 DEG C, and Keep agitation reaction 5 ~ 10min obtains potassium magnesium sulfate slip.
(4) crushing drying is cooled:
Opening reactor discharge valve is put in stock pan by molten for the potassium magnesium sulfate of generation slurry, and be crushed to below 1mm after naturally cooling solidifies, oven drying at low temperature obtains potassium magnesium sulfate fertilizer product.
Embodiment 3:
(1) sal enixum slip is prepared:
The 123.8Kg vitriol oil (H is added in reactor 2sO 4mass content 95%), stir and reacting by heating still to 140 DEG C, then in reactor, add 106.4Kg Klorvess Liquid (KCl mass content 70%), keep reactor temperature to be 140 DEG C of Keep agitation 60min, hydrogen chloride gas is all overflowed, obtains sal enixum slip 193.7Kg(KHSO 4mass content 70.2%).
(2) magnesium oxide slip is prepared:
In plastic tank, add 40Kg magnesium oxide and 80Kg clear water, stir preparation and obtain magnesium oxide slip 120Kg (MgO mass content 33.2%) for subsequent use.
(3) neutralization reaction:
The magnesium oxide slip of (2) being joined joins in the sal enixum slip of (1) gained, reacting by heating still temperature to 160 DEG C, and Keep agitation reaction 5 ~ 10min obtains potassium magnesium sulfate slip.
(4) crushing drying is cooled:
Opening reactor discharge valve is put in stock pan by molten for the potassium magnesium sulfate of generation slurry, and be crushed to below 1mm after naturally cooling solidifies, oven drying at low temperature obtains potassium magnesium sulfate fertilizer product.
The potash magnesium sulphate fertilizer inspection method specified in GB/T20937-2007 detects, and the index of the potash magnesium sulphate fertilizer that embodiment 1-3 obtains is as shown in the table:
As can be known from the above table, the potassium magnesium sulfate product prepared through the inventive method all reaches potash magnesium sulphate fertilizer national standard (GB/T20937-2007) acceptable end product standard.

Claims (5)

1. the production method of a potash magnesium sulphate fertilizer, it is characterized in that: it with Repone K, the vitriol oil and magnesium oxide for raw material, Repone K and strong sulfuric acid response obtain sal enixum slip, sal enixum slip obtains potassium magnesium sulfate slip with magnesium oxide slip again, and namely potassium magnesium sulfate slip obtains potash magnesium sulphate fertilizer through cooling, fragmentation, baking operation.
2. the production method of a kind of potash magnesium sulphate fertilizer according to claim 1, is characterized in that: the preparation method of described potassium magnesium sulfate slip comprises the following steps:
Prepare sal enixum slip: potassium chloride and vitriol oil mix and blend react 30-60min, hydrogen chloride gas is overflowed to obtain sal enixum slip, and wherein control temperature of reaction 80 ~ 140 DEG C, the mol ratio of Repone K and the vitriol oil is with KCl and H 2sO 4count 1:1 ~ 1.2;
(2) magnesium oxide slip is prepared: according to quality than magnesium oxide: water=1:0.5 ~ 2, magnesium oxide is mixed obtained magnesium oxide slip with water;
(3) potassium magnesium sulfate slip is prepared: the sal enixum slip obtained by step (1) and the magnesium oxide slip Hybrid Heating of step (2) are reacted 5 ~ 10min and namely obtained potassium magnesium sulfate slip, wherein controlling temperature of reaction is 120 ~ 160 DEG C, and the mol ratio of sal enixum slip and magnesium oxide slip is with KHSO 41:1 is got with MgO meter.
3. the production method of a kind of potash magnesium sulphate fertilizer according to claim 2, is characterized in that: described in step (1), Repone K mixes with the vitriol oil in the form of a solution, wherein concentration >=50% of Klorvess Liquid.
4. the production method of a kind of potash magnesium sulphate fertilizer according to claim 2, is characterized in that: concentration >=90% of the vitriol oil described in step (1).
5. the production method of a kind of potash magnesium sulphate fertilizer according to claim 2, is characterized in that: the hydrogen chloride gas grading absorption that described step (1) is overflowed makes hydrochloric acid.
CN201410526143.6A 2014-10-09 2014-10-09 Production method of potash magnesium sulfate fertilizer Pending CN104311164A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060329A (en) * 2015-08-03 2015-11-18 茫崖兴元钾肥有限责任公司 Method for producing picromerite by taking potassium chloride and mirabilite as raw materials
CN107827127A (en) * 2017-12-04 2018-03-23 青海中航资源有限公司 A kind of method that potassium sulfate Water soluble fertilizer is produced using low grade potassium ore deposit
CN107954453A (en) * 2017-12-14 2018-04-24 龙蟒大地农业有限公司 A kind of method for preparing large-particle potassium sulfate magnesium crystal and little particle potassium sulfate crystal
CN109650947A (en) * 2019-02-15 2019-04-19 夏念冉 A kind of method of industrial waste sulfuric acid production hydrogen sulfate potash fertilizer
EP4166526A1 (en) * 2021-10-15 2023-04-19 Yara International ASA Method for producing a potassium-containing fertilizer with a low content of water-insoluble material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1155528A (en) * 1996-07-11 1997-07-30 南开大学 Preparation of potassium-magnesium alum
CN1197039A (en) * 1997-04-23 1998-10-28 张振文 One-step process for prodn. of farm potassium sulphate
CN102765994A (en) * 2012-08-15 2012-11-07 上海化工研究院 Method for preparing granular potash fertilizer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1155528A (en) * 1996-07-11 1997-07-30 南开大学 Preparation of potassium-magnesium alum
CN1197039A (en) * 1997-04-23 1998-10-28 张振文 One-step process for prodn. of farm potassium sulphate
CN102765994A (en) * 2012-08-15 2012-11-07 上海化工研究院 Method for preparing granular potash fertilizer

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060329A (en) * 2015-08-03 2015-11-18 茫崖兴元钾肥有限责任公司 Method for producing picromerite by taking potassium chloride and mirabilite as raw materials
CN107827127A (en) * 2017-12-04 2018-03-23 青海中航资源有限公司 A kind of method that potassium sulfate Water soluble fertilizer is produced using low grade potassium ore deposit
CN107954453A (en) * 2017-12-14 2018-04-24 龙蟒大地农业有限公司 A kind of method for preparing large-particle potassium sulfate magnesium crystal and little particle potassium sulfate crystal
CN109650947A (en) * 2019-02-15 2019-04-19 夏念冉 A kind of method of industrial waste sulfuric acid production hydrogen sulfate potash fertilizer
EP4166526A1 (en) * 2021-10-15 2023-04-19 Yara International ASA Method for producing a potassium-containing fertilizer with a low content of water-insoluble material
WO2023062176A1 (en) * 2021-10-15 2023-04-20 Yara International Asa Method for producing a potassium-containing fertilizer with a low content of water-insoluble material

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