CN1098702A - Production of potashsium sulfate with assistant method - Google Patents
Production of potashsium sulfate with assistant method Download PDFInfo
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- CN1098702A CN1098702A CN 93109812 CN93109812A CN1098702A CN 1098702 A CN1098702 A CN 1098702A CN 93109812 CN93109812 CN 93109812 CN 93109812 A CN93109812 A CN 93109812A CN 1098702 A CN1098702 A CN 1098702A
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- tartar
- vitriolate
- sulfate
- mother liquor
- potashsium
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Abstract
The present invention is a kind of novel process of production of potashsium sulfate with assistant method, and it is to produce vitriolate of tartar with Repone K and ammonium sulfate metathesis, and the adding organic additive further precipitates, separates vitriolate of tartar, auxiliary agent recycling use, side product sodium chloride in its mother liquor.The time of adopting the present invention can shorten reaction also can be brought up to the yield of vitriolate of tartar more than 95% from 60%, according to this explained hereafter vitriolate of tartar, the metathetic reaction times shortens greatly, and the quality of vitriolate of tartar reaches the standard of top grade product and first grade among the potassium sulfate for agricultural use specialized standard ZBG21006-89 of the People's Republic of China (PRC).
Description
The present invention is a kind of method of utilizing Repone K and ammonium sulfate to produce potassium product, belongs to the field of Chemicals processing.
Vitriolate of tartar is a kind of important chemical material, also is the main source of potassium element in the chlorideless potassic fertilizer, and especially demand is very big in the composite fertilizer of cash crop such as flue-cured tobacco, oranges and tangerines, grape, tealeaves, so the production economic implications of vitriolate of tartar is very big.The method of producing vitriolate of tartar in the prior art is a lot, wherein a class is to be raw material with Repone K (KO content＞60%) and sulfuric acid amine (containing N about 21%), prepare vitriolate of tartar through replacement(metathesis)reaction, thereby but owing to adopt different technology to obtain the vitriolate of tartar of different qualities.Method as China chemical research unit is: according to the reaction solution that calculates the formulated definite composition, add Repone K and ammonium sulfate again and stir certain hour down in 60 ℃, slip after reaction is finished filters with D=110mm porcelain pore funnel, filter cake is used a certain amount of water washing again, gets the vitriolate of tartar finished product at last; KO only 46.31% and nitrogenous (N) about 2.9% in the potassium product that obtains with this method, when mother liquid evaporation is separated out ammonium chloride crystals, the vitriolate of tartar that is dissolved in wherein also will be separated out simultaneously, therefore a large amount of potassium remains in the ammonium chloride, wherein KO about 23%, N is about 15%, and this has caused the reduction of vitriolate of tartar yield.
These problems in view of the prior art existence, the objective of the invention is to: the novel process that a kind of production of potashsium sulfate with assistant method is provided, produce vitriolate of tartar with Repone K and ammonium sulfate metathesis, in its mother liquor, add the further precipitate and separate vitriolate of tartar of organic additive then, the auxiliary agent recycling use is paid and is produced ammonium chloride; The time of adopting the present invention can shorten reaction also can be brought up to the yield of vitriolate of tartar more than 95% from 60%.
The present invention constitutes like this: a, raw material Repone K and ammonium sulfate are made solution near saturation concentration respectively, removed by filter mechanical impurity; B, under the agitation condition two kinds of solution are mixed in reactive tank in 60～100 ℃, after vitriolate of tartar was separated out, the cooling mother liquor was further separated out vitriolate of tartar to room temperature; C, centrifugation go out vitriolate of tartar and dry potassium product; The organic additive that at room temperature adds 0.2～3 times of its volume after remaining mother liquor by volume measures after d, the centrifugation, treat that the vitriolate of tartar mass crystallization is separated out after, recentrifuge is isolated vitriolate of tartar and is dried and obtains potassium product; The mother liquor that e, evaporation stay at last must be paid product ammonium chloride, isolates organic additive recirculation behind steam cooling fractionation or the vaporize water and uses; Used in the present invention organic additive be dissolved in water alcohols and (or) Oxygenic heterocyclic compounds.
Concrete technological process is:
1, according to reaction formula 2KCl+(NH) SO=KSO+2NHCl and material purity, calculate the raw material consumption, under 60～100 ℃ of temperature, they are made solution respectively near saturation concentration, again solution is removed by filter mechanical impurity.
2, in reactive tank two kinds of solution are mixed under 60～100 ℃ of agitation conditions, because the solubleness of vitriolate of tartar is little, its crystallization is immediately separated out, and the cooling mother liquor allows more vitriolate of tartar crystallization separate out to room temperature.
3, reaction mass is emitted from reactive tank, isolate vitriolate of tartar and drying, get potassium product through whizzer.
4, Yu Xia mother liquor is sent into settling bath, presses the mother liquor volume metering, adds the organic additive of 0.2～3 times of its volume under the room temperature, stirs; Because the adding of auxiliary agent has changed the constitutional features of solvent in the mother liquor, thereby the vitriolate of tartar mass crystallization is separated out, recentrifuge is isolated vitriolate of tartar and is dried.In the present invention, the auxiliary agent of use is water-soluble alcohols and Oxygenic heterocyclic compounds.
5, evaporate the mother liquor that stays at last, obtain paying a product ammonium chloride, from the steam that evaporates, fractionate out auxiliary agent, or isolate auxiliary agent behind the transpiring moisture, auxiliary agent is recycled through cooling.
According to this explained hereafter vitriolate of tartar, the yield of its vitriolate of tartar can reach more than 95% the ratio of theoretical amount (the real receipts amount of vitriolate of tartar with) and the metathetic reaction times shortens greatly; The quality of vitriolate of tartar reaches the standard of top grade product and first grade among the potassium sulfate for agricultural use specialized standard ZBG21006-89 of the People's Republic of China (PRC).
Embodiments of the invention 1: with ethanol is auxiliary agent.
In the time of 90 ℃, 400g ammonium sulfate is dissolved in the 460ml water, and in the time of 90 ℃, 452g Repone K is dissolved in the 940ml water, and two solution are in 90 ℃ of mixing then, and vitriolate of tartar is that crystallization is separated out, the reactant cool to room temperature, and filtering separation gets vitriolate of tartar and mother liquor I; In the mother liquor I, add 1400ml ethanol (making auxiliary agent) again, at this moment have potassium sulfate crystal to separate out again, filter mother liquor II and potassium sulfate crystal.Wash vitriolate of tartar, the dry finished product vitriolate of tartar that gets with water.The mother liquid evaporation II reclaims ethanol and the evaporate to dryness mother liquor gets solid ammonium chloride, and twice crystalline sulfuric acid potassium adds up to yield more than 95%.
Embodiments of the invention 2: with methyl alcohol is auxiliary agent.
In the time of 90 ℃, 400g ammonium sulfate is dissolved in the 460ml water, and in the time of 90 ℃, 452g Repone K is dissolved in the 940ml water, and two solution are in 90 ℃ of mixing then, and vitriolate of tartar is that crystallization is separated out, the reactant cool to room temperature, and filtering separation gets vitriolate of tartar and mother liquor I; In the mother liquor I, add 1400ml methyl alcohol (making auxiliary agent) again, at this moment have potassium sulfate crystal to separate out again, filter mother liquor II and potassium sulfate crystal.Wash vitriolate of tartar, the dry finished product vitriolate of tartar that gets with water.The mother liquid evaporation II reclaims methyl alcohol and the evaporate to dryness mother liquor gets solid ammonium chloride, and twice crystalline sulfuric acid potassium adds up to yield more than 95%.
Claims (2)
1, production of potashsium sulfate with assistant method is characterized in that:
A, raw material Repone K and ammonium sulfate are made solution near saturation concentration respectively, removed by filter mechanical impurity;
B, under the agitation condition two kinds of solution are mixed in reactive tank in 60～100 ℃, after vitriolate of tartar was separated out, the cooling mother liquor was further separated out vitriolate of tartar to room temperature;
C, centrifugation go out vitriolate of tartar and dry potassium product;
The organic additive that at room temperature adds 0.2～3 times of its volume after d, the centrifugation behind the remaining mother liquor ammonium volume metering, treat that the vitriolate of tartar mass crystallization is separated out after, recentrifuge is isolated vitriolate of tartar and is dried and obtains potassium product;
The mother liquor that e, evaporation stay at last must be paid product ammonium chloride, isolates organic additive recirculation behind steam cooling fractionation or the vaporize water and uses.
2, according to the described production of potashsium sulfate with assistant method of claim 1, it is characterized in that: used organic additive be dissolved in water alcohols and (or) Oxygenic heterocyclic compounds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93109812 CN1098702A (en) | 1993-08-13 | 1993-08-13 | Production of potashsium sulfate with assistant method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93109812 CN1098702A (en) | 1993-08-13 | 1993-08-13 | Production of potashsium sulfate with assistant method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1098702A true CN1098702A (en) | 1995-02-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93109812 Pending CN1098702A (en) | 1993-08-13 | 1993-08-13 | Production of potashsium sulfate with assistant method |
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| CN (1) | CN1098702A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042918C (en) * | 1995-08-01 | 1999-04-14 | 化学工业部长沙化学矿山设计研究院 | One-step method for preparing potassium sulfate |
| CN102703689A (en) * | 2012-06-14 | 2012-10-03 | 沈阳化工大学 | Process method for extracting and separating iron from industrial waste iron mud and preparing iron oxide red |
| CN104118890A (en) * | 2014-08-06 | 2014-10-29 | 柳仁民 | Method for producing potassium (sodium) sulfate at low temperature |
| CN104261433A (en) * | 2014-09-24 | 2015-01-07 | 湘潭市天志科技有限公司 | Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste |
| CN107417307A (en) * | 2017-09-12 | 2017-12-01 | 化工部长沙设计研究院 | A kind of preparation technology of water-soluble drip irrigation potassium sulfate |
| CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
-
1993
- 1993-08-13 CN CN 93109812 patent/CN1098702A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042918C (en) * | 1995-08-01 | 1999-04-14 | 化学工业部长沙化学矿山设计研究院 | One-step method for preparing potassium sulfate |
| CN102703689A (en) * | 2012-06-14 | 2012-10-03 | 沈阳化工大学 | Process method for extracting and separating iron from industrial waste iron mud and preparing iron oxide red |
| CN104118890A (en) * | 2014-08-06 | 2014-10-29 | 柳仁民 | Method for producing potassium (sodium) sulfate at low temperature |
| CN104261433A (en) * | 2014-09-24 | 2015-01-07 | 湘潭市天志科技有限公司 | Method for producing potassium sulfate from potassium/chlorine-ion-containing solid waste |
| CN104261433B (en) * | 2014-09-24 | 2016-06-29 | 湘潭市天志科技有限公司 | A kind of method that solid waste utilized containing potassium, chloride ion produces potassium sulfate |
| CN107417307A (en) * | 2017-09-12 | 2017-12-01 | 化工部长沙设计研究院 | A kind of preparation technology of water-soluble drip irrigation potassium sulfate |
| CN109911919A (en) * | 2017-12-13 | 2019-06-21 | 北京恩泽佳立科技有限公司 | Potassium sulfate preparation system and method |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |