CN101434402A - Method of producing potassium sulfate by reaction, extraction and crystallization one-step method - Google Patents
Method of producing potassium sulfate by reaction, extraction and crystallization one-step method Download PDFInfo
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- CN101434402A CN101434402A CNA200710114514XA CN200710114514A CN101434402A CN 101434402 A CN101434402 A CN 101434402A CN A200710114514X A CNA200710114514X A CN A200710114514XA CN 200710114514 A CN200710114514 A CN 200710114514A CN 101434402 A CN101434402 A CN 101434402A
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Abstract
The invention relates to the new process for producing lemery by a one-step method of reaction-extraction-crystallization, which takes dilute sulphuric acid and potassium chloride as the raw material and adopts the one-step reaction of a complex extracting agent to extract and crystallize to prepare the lemery under normal temperature; the three processes of reaction, extraction and crystallization are simultaneously carried out in a same device, and the solid lemery can be obtained without heating and compression. The used extracting agent can be effectively recovered by the back extraction of ammonia so as to be reused. The whole process is a closed cycle, which ensures zero discharge of three wastes.
Description
Technical field
The present invention relates to chemical field, particularly reaction, extraction and crystallization-footwork is produced the method for vitriolate of tartar.
Background technology
Vitriolate of tartar is the principal item of chlorideless potassic fertilizer, is specially adapted to avoid the cash crop such as tealeaves, tobacco, carbohydrate and fruit of chlorine.The proportion of production of present nitrogenous fertilizer of China and phosphate fertilizer can be fit to the demand of agriculture production development substantially, but the breach of potash fertilizer is increasing, especially vitriolate of tartar.At present industrially produce vitriolate of tartar from Repone K 3 kinds of methods are arranged: double decomposition, form the Mannheim proeess of company on the Taiwan green grass or young crops of the method for putting and introduction, wherein the double decomposition transformation efficiency is low, and quality product is difficult to control; Form and put the method less investment, cost is low, quality product is high, but easy salt crust, obstruction during suitability for industrialized production makes the production operation serialization very difficult; As for Mannheim proeess, then need at high temperature carry out, a complete set of equipment is introduction, the production domesticization difficulty, equipment corrosion is serious, investment big (the ton device need be invested about 3,500 ten thousand yuan), the cost height, a large amount of hydrochloric acid of by-product have waste residue, spent acid to be difficult for handling in addition.
Summary of the invention
Vitriolate of tartar production new technology of the present invention, the novel process that the reaction, extraction and crystallization single stage method is produced vitriolate of tartar has been proposed, be raw material promptly with dilute sulphuric acid and Repone K, adopt composite extractant single step reaction extractive crystallization to produce vitriolate of tartar at normal temperatures, reaction, extraction and 3 processes of crystallization are carried out in same equipment simultaneously, need not the concentrated solid sulphuric acid potassium that promptly gets of heating.Used extraction agent can reclaim extraction agent so that reuse effectively through the ammoniacal liquor back extraction.Whole process closed cycle, basic three-waste free discharge.
The potassium product that the present invention seeks to make meets the quality standard of GB premium grads, and the byproduct ammonia chloride meets the nitrogen fertilizer in agriculture standard.
Technical scheme of the present invention is
The reaction, extraction and crystallization single stage method is produced the novel process of vitriolate of tartar, be raw material promptly with dilute sulphuric acid and Repone K, adopt composite extractant single step reaction extractive crystallization to produce vitriolate of tartar at normal temperatures, reaction, extraction and 3 processes of crystallization are carried out in same equipment simultaneously, need not the concentrated solid sulphuric acid potassium that promptly gets of heating.
Technique effect
Reaction, extraction and crystallization single stage method production potassium sulfate process flow process is simple, and less investment is carried out under the normal temperature and pressure, avoids reaction under the vitriol oil, easy to operate, the extraction agent loss is few, the solution closed cycle, basic three-waste free discharge meets eco-friendly requirement, is a kind of green chemical industry technology.Major product vitriolate of tartar and byproduct purity of ammonia chloride height, return on investment is also high.Technology is not high to ingredient requirement, and adaptability is strong, as sulfur acid or contain potassium waste water, can adopt yet, and therefore, with double decomposition, Mannheim proeess with form the method for putting and compare, novel process has significant advantage to have a bright future.
Embodiment:
1, the preparation of raw material operation is evacuated to test tank with potassium sulfate mother liquid, adds thinning tank after metering, adds the vitriol oil while stirring, then is evacuated in the preparing tank with acid proof pump, begins to stir, and drops into solid potassium chloride and the adding water through metering, continues to stir.Filter by plate-and-frame filter press with acid proof pump then, filtrate is used for extractive reaction, and filter cake is calcium sulfate, the sal epsom precipitation that solid insoluble in the raw material Repone K and Ca2+ wherein, Mg2+ and sulfuric acid generate.The filtration of preparation liquid not only can improve the purity of product vitriolate of tartar, also can reduce the waste of machine solvent recklessly.Present method has avoided 98% the vitriol oil directly to contact with organic phase, prevents that effectively organic phase is sulfonated or oxidation, guarantees that organic solvent can long-term operation, simultaneously the vitriol oil is directly contacted with solid potassium chloride, prevents the local hydrogen chloride gas that produces.
2, the organic solvent of extraction process through reclaiming is evacuated in the extractive crystallization reactor, the preparation of suction while stirring liquid, fully carrying out profit after the reaction is separated, oil phase removes to reclaim extraction agent to the reextraction operation, separate the water obtain and solid phase through centrifugation, dry, crush and screen and can get high-quality vitriolate of tartar finished product.Organic phase need regularly measure and add into fresh organic solvent.
3, reextraction operation has hydrochloric acid and a small amount of vitriolic organic solvent contact reacts with ammoniacal liquor and load, and ammoniacal liquor back extraction effectively goes out hydrochloric acid and sulfuric acid, and the ammonium chloride and the ammonium sulfate precipitation of generation come out, and carry out profit then and are separated, and organic phase is to extraction process.Water and solid phase are after centrifugation, and be dry, crush and screen and can get nitrogen fertilizer in agriculture.
Claims (3)
1, the reaction, extraction and crystallization single stage method is produced the method for vitriolate of tartar, it is characterized in that adopting at normal temperatures composite extractant single step reaction extractive crystallization to produce vitriolate of tartar, reaction, extraction and 3 processes of crystallization are carried out in same equipment simultaneously, need not the concentrated solid sulphuric acid potassium that promptly gets of heating.
2, reaction, extraction and crystallization single stage method as claimed in claim 1 is produced the method for vitriolate of tartar, it is characterized in that the organic solvent of extraction process through reclaiming is evacuated in the extractive crystallization reactor, the preparation of suction while stirring liquid, fully carrying out profit after the reaction is separated, oil phase removes to reclaim extraction agent to the reextraction operation, separate the water obtain and solid phase through centrifugation, dry, crush and screen and can get high-quality vitriolate of tartar finished product.
3, reaction, extraction and crystallization single stage method as claimed in claim 1 is produced the method for vitriolate of tartar, the operation that it is characterized in that stripping has hydrochloric acid and a small amount of vitriolic organic solvent contact reacts with ammoniacal liquor and load, ammoniacal liquor back extraction effectively goes out hydrochloric acid and sulfuric acid, the ammonium chloride and the ammonium sulfate precipitation that generate come out, carry out profit then and be separated, organic phase is to extraction process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710114514XA CN101434402A (en) | 2007-11-13 | 2007-11-13 | Method of producing potassium sulfate by reaction, extraction and crystallization one-step method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710114514XA CN101434402A (en) | 2007-11-13 | 2007-11-13 | Method of producing potassium sulfate by reaction, extraction and crystallization one-step method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101434402A true CN101434402A (en) | 2009-05-20 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200710114514XA Pending CN101434402A (en) | 2007-11-13 | 2007-11-13 | Method of producing potassium sulfate by reaction, extraction and crystallization one-step method |
Country Status (1)
| Country | Link |
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| CN (1) | CN101434402A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896683A (en) * | 2014-04-14 | 2014-07-02 | 国投新疆罗布泊钾盐有限责任公司 | Water-soluble instant potassium sulfate fertilizer |
| CN108083298A (en) * | 2018-01-15 | 2018-05-29 | 东南大学 | It is a kind of to prepare the nanocrystalline method of potassium sulfate |
| CN111960439A (en) * | 2020-08-31 | 2020-11-20 | 四川轻化工大学 | Novel extraction crystallization method for preparing potassium sulfate crystal, fluidization device and application thereof |
-
2007
- 2007-11-13 CN CNA200710114514XA patent/CN101434402A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896683A (en) * | 2014-04-14 | 2014-07-02 | 国投新疆罗布泊钾盐有限责任公司 | Water-soluble instant potassium sulfate fertilizer |
| CN103896683B (en) * | 2014-04-14 | 2015-09-30 | 国投新疆罗布泊钾盐有限责任公司 | Water-soluble instant potassium sulfate fertilizer |
| CN108083298A (en) * | 2018-01-15 | 2018-05-29 | 东南大学 | It is a kind of to prepare the nanocrystalline method of potassium sulfate |
| CN111960439A (en) * | 2020-08-31 | 2020-11-20 | 四川轻化工大学 | Novel extraction crystallization method for preparing potassium sulfate crystal, fluidization device and application thereof |
| CN111960439B (en) * | 2020-08-31 | 2022-11-15 | 四川轻化工大学 | Extraction crystallization method for preparing potassium sulfate crystal, fluidizing device and application thereof |
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Open date: 20090520 |