CN102633537A - Method for producing watersoluble potassium sulfate - Google Patents
Method for producing watersoluble potassium sulfate Download PDFInfo
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- CN102633537A CN102633537A CN2012101201155A CN201210120115A CN102633537A CN 102633537 A CN102633537 A CN 102633537A CN 2012101201155 A CN2012101201155 A CN 2012101201155A CN 201210120115 A CN201210120115 A CN 201210120115A CN 102633537 A CN102633537 A CN 102633537A
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Abstract
The invention relates to a method for producing fully-watersoluble potassium sulfate. The method comprises the steps of reacting sulfuric acid and potassium chloride in a mole ratio of (1.05-1.15):1 at a temperature of 110-130 DEG C to generate a potassium bisulfate fused solution; adding water for diluting the potassium bisulfate fused solution to specific gravity of 1.40-1.45g/ml, so as to prepare a potassium bisulfate solution with a mass concentration being 35-40%; controlling the temperature at about 80 DEG C; filtering the potassium bisulfate solution to removing insoluble impurities; adding urea in the potassium bisulfate solution in a mole ratio of 1:(1.2-1.3) of the urea to the added sulfuric acid as reference to the amount of the added urea; reacting for an hour at the temperature of 70-80 DEG C; and after cooling crystallization and centrifugal separation, so as to obtain crystal potassium sulfate. The method has the following advantages: the materials have extensive sources and are cheap and easy to obtain; the technical flow is simple and convenient to operate; and the utilization rate of potassium can be up to over 99%, and the emission of three wastes (waste gas, waste water and waste residues) can be avoided.
Description
Technical field
The invention belongs to water-soluble fertile production field, specifically a kind of method with agricultural potassium chloride, industrial sulphuric acid and the complete water-soluble vitriolate of tartar of agricultural urea production.
Background technology
The main method of producing vitriolate of tartar at present both at home and abroad is a Mannheim proeess; This method be with 98% the vitriol oil at high temperature with Repone K direct reaction in mannheim furnace, at first at a lower temperature, sulfuric acid and Repone K reaction; Produce sal enixum; Under comparatively high temps, sal enixum and Repone K reaction generate vitriolate of tartar then, and its output accounts for more than 50%.The advantage of this method is that production technology is ripe, and technological process is comparatively simple, and the product vitriolate of tartar is of high grade, and the potassium yield is higher, and shortcoming is that cost of raw and processed materials is high because reaction is in the condition of high temperature strong acid, and equipment corrosion is serious, and maintenance capacity is big.Other working method can be divided into two big types substantially: the one, from sulfate-type sea lake salt bittern and subsurface brine, extract; The method of main utilization has: high temp. salt method, flotation process, vortex method, solvay liquor and Bittern of Salt Pan ammonia process, liquid-film method etc.; This method exists investment higher; Cost of equipment is bigger, and flow process is longer, and flotation reagent has certain shortcomings such as influence to the quality of product.The 2nd, get with the solid kalium mine of puritan filler potassium ore or complex component is made of stones, promptly utilize the ore contain potassium vitriol to obtain vitriolate of tartar, defective such as this method exists that the separating treatment difficulty is big, poor product quality, yield are low through series of physical, chemical transformation.The method of therefore inventing a kind of new complete water-soluble vitriolate of tartar of production is highly profitable.
Summary of the invention
The objective of the invention is defective, a kind of method with agricultural potassium chloride, industrial sulphuric acid and the complete water-soluble vitriolate of tartar of agricultural urea production is provided to existing production Technique of Potassium Sulphate.
To achieve these goals, the present invention adopts following technical scheme:
It is earlier with sulfuric acid and Repone K 1.05-1.15 in molar ratio: 1, under 110-130 ℃ of temperature, react generation sal enixum molten mass, and be 1.40-1.45g/ml with sal enixum molten mass thin up to proportion then; Be mixed with the potassium hydrogen sulfate solution that mass concentration is 35-40%; Temperature is controlled at about 80 ℃, removes by filter insoluble impurities, in potassium hydrogen sulfate solution, adds urea again; The add-on of urea adds vitriolic mol ratio 1: 1.2-1.3 according to urea and institute and adds; 70-80 ℃ of down reaction one hour, pass through crystallisation by cooling and spinning then after, obtain the lenticular vitriolate of tartar.Mode through adding urea can promote separating out of lenticular vitriolate of tartar, saves N-process.
Butt potassium oxide>=52% of gained lenticular vitriolate of tartar wherein, chlorine root≤0.2%, water-insoluble≤0.1%, moisture content≤3%.Wherein Repone K and the sulfuric acid quality percentage composition as raw material is respectively 90-95% Repone K, 98% industrial sulphuric acid.
The lenticular vitriolate of tartar that the present invention produces can be used as water soluble potassic fertilizer separately, also can be used as the intermediate raw material of producing water soluble fertilizer.The hydrogen chloride gas body and function de-salted water that produces in the reaction process absorbs processes 31% hydrochloric acid sub product, and the mother liquor after centrifugal returns composite fertilizer's system recoveries utilization.
The present invention is with low side raw material 90-95% agricultural potassium chloride, 98% industrial sulphuric acid and agricultural urea, produces the novel technique route of full water-soluble vitriolate of tartar through the method for chemosynthesis.
Adopt the present invention that following advantage is arranged:
1, can be raw material with agricultural potassium chloride, industrial sulphuric acid and agricultural urea directly, raw material sources are extensive, and be cheap and easy to get;
2, technical process is simple, and is easy to operate, and temperature of reaction is low, and energy consumption is low, and low to the equipment material requirement, one-time investment is few;
3, can directly obtain full water-soluble crystal vitriolate of tartar, added value is high;
4, the hydrogen chloride gas that produces can be made into 31% hydrochloric acid sub product, and slag that produces in the production process and mother liquor return composite fertilizer's system recoveries utilization, and the utilization ratio of potassium can be up to more than 99%, and three-waste free discharge belongs to environmental protection technology.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
Below in conjunction with embodiment the present invention is done to further describe, following embodiment only is to concrete elaboration of the present invention, does not limit protection scope of the present invention:
Embodiment one:
1, the vitriol oil of quality percentage composition 98% and 90% Repone K were dropped into the sal enixum reactive tank in 1.15: 1 in molar ratio; Under 110 ℃ of temperature, react; Generate sal enixum molten mass and hydrogen chloride gas, hydrogenchloride is taken away after absorption system absorbs with de-salted water and is obtained 31% hydrochloric acid sub product;
2, the sal enixum molten mass that reaction is good is delivered to dilution trap, and to be diluted with water to proportion be 1.40g/ml; Potassium hydrogen sulfate solution (the containing small-amount free sulfuric acid) controlled temperature that is mixed with concentration about 40% is about 80 ℃; And then will dilute good potassium hydrogen sulfate solution and be sent to strainer and filter; Remove water-insoluble impurity wherein, filter the back potassium hydrogen sulfate solution and flow into reactive tank, recoil slag slurry is sent to mother liquid tank and returns the composite fertilizer system;
3, in potassium hydrogen sulfate solution, add urea, the add-on of urea adds the vitriolic mol ratio and adds at 1: 1.25 with institute according to urea, control reaction temperature 70-80 ℃, reacts and is sent to the crystallisation by cooling groove after one hour and carries out crystallisation by cooling;
When 4, feed temperature is reduced to 35 ℃ of left and right sides in the crystallizer tank to be cooled, feed liquid is sent to whizzer, the potassium sulfate crystal that gets product after the separation, the mother liquor of generation is sent to mother liquid tank and returns the composite fertilizer system.Butt potassium oxide>=52% of gained lenticular vitriolate of tartar, chlorine root≤0.2%, water-insoluble≤0.1%, moisture content≤3%.
Aforementioned production method is applicable to the composite fertilizer manufacturing enterprise of certain scale; The slag and the mother liquor that produce in process of production for the ease of digestion during actual production; Need to rely on composite fertilizer's production equipment of certain scale, realize whole useful matter recyclings, make its maximization of economic benefit; Common fertilizer enterprise can enrich product through the complete water-soluble vitriolate of tartar of coproduction the kind and the raising competitiveness of product in market improve economic benefit of enterprises to greatest extent through optimizing and combining of resource.
Press aforementioned production method; To produce 1 ton of butt potassium oxide>=52%, chlorine root≤0.2%, water-insoluble≤0.1%; The lenticular potassium product of moisture content≤3% is an example, and the economic benefit that is produced is calculated like following table (raw material, finished product and sub product all calculate by the existing market valency):
Can find out from the data of calculating, composite fertilizer manufacturing enterprise of certain scale carried out the technological transformation of coproduction full water-soluble vitriolate of tartar, can obtain remarkable economic efficiency according to the present invention.
Embodiment two:
1, the vitriol oil of quality percentage composition 98% and 95% Repone K were dropped into the sal enixum reactive tank in 1.05: 1 in molar ratio; Under 130 ℃ of temperature, react; Generate sal enixum molten mass and hydrogen chloride gas, hydrogenchloride is taken away after absorption system absorbs with de-salted water and is obtained 31% hydrochloric acid sub product;
2, the sal enixum molten mass that reaction is good is delivered to dilution trap, and to be diluted with water to proportion be 1.45g/ml; Potassium hydrogen sulfate solution (the containing small-amount free sulfuric acid) controlled temperature that is mixed with concentration about 40% is about 80 ℃; And then will dilute good potassium hydrogen sulfate solution and be sent to strainer and filter; Remove water-insoluble impurity wherein, filter the back potassium hydrogen sulfate solution and flow into reactive tank, recoil slag slurry is sent to mother liquid tank and returns the composite fertilizer system;
3, in potassium hydrogen sulfate solution, add urea, the add-on of urea adds the vitriolic mol ratio and adds at 1: 1.30 with institute according to urea, control reaction temperature 70-80 ℃, reacts and is sent to the crystallisation by cooling groove after one hour and carries out crystallisation by cooling;
When 4, feed temperature is reduced to 35 ℃ of left and right sides in the crystallizer tank to be cooled, feed liquid is sent to whizzer, the potassium sulfate crystal that gets product after the separation, the mother liquor of generation is sent to mother liquid tank and returns the composite fertilizer system.Butt potassium oxide>=52% of gained lenticular vitriolate of tartar, chlorine root≤0.2%, water-insoluble≤0.1%, moisture content≤3%.
Embodiment three:
1, the vitriol oil of quality percentage composition 98% and 93% Repone K were dropped into the sal enixum reactive tank in 1.10: 1 in molar ratio; Under 120 ℃ of temperature, react; Generate sal enixum molten mass and hydrogen chloride gas, hydrogenchloride is taken away after absorption system absorbs with de-salted water and is obtained 31% hydrochloric acid sub product;
2, the sal enixum molten mass that reaction is good is delivered to dilution trap, and to be diluted with water to proportion be 1.45g/ml; Potassium hydrogen sulfate solution (the containing small-amount free sulfuric acid) controlled temperature that is mixed with concentration about 40% is about 80 ℃; And then will dilute good potassium hydrogen sulfate solution and be sent to strainer and filter; Remove water-insoluble impurity wherein, filter the back potassium hydrogen sulfate solution and flow into reactive tank, recoil slag slurry is sent to mother liquid tank and returns the composite fertilizer system;
3, in potassium hydrogen sulfate solution, add urea, the add-on of urea adds the vitriolic mol ratio and adds at 1: 1.20 with institute according to urea, control reaction temperature 70-80 ℃, reacts and is sent to the crystallisation by cooling groove after one hour and carries out crystallisation by cooling;
When 4, feed temperature is reduced to 35 ℃ of left and right sides in the crystallizer tank to be cooled, feed liquid is sent to whizzer, the potassium sulfate crystal that gets product after the separation, the mother liquor of generation is sent to mother liquid tank and returns the composite fertilizer system.Butt potassium oxide>=52% of gained lenticular vitriolate of tartar, chlorine root≤0.2%, water-insoluble≤0.1%, moisture content≤3%.
Claims (3)
1. method of producing complete water-soluble vitriolate of tartar, it is earlier with sulfuric acid and Repone K 1.05-1.15 in molar ratio: 1, under 110-130 ℃ of temperature, react generation sal enixum molten mass; Be 1.40-1.45g/ml with sal enixum molten mass thin up to proportion then, be mixed with the potassium hydrogen sulfate solution that mass concentration is 35-40%, temperature is controlled at about 80 ℃; Remove by filter insoluble impurities; In potassium hydrogen sulfate solution, add urea again, the add-on of urea adds vitriolic mol ratio 1: 1.2-1.3 according to urea with institute and adds, and reacts one hour down at 70-80 ℃; After passing through crystallisation by cooling and spinning then, obtain the lenticular vitriolate of tartar.
2. a kind of method of producing complete water-soluble vitriolate of tartar according to claim 1, butt potassium oxide>=52% of gained lenticular vitriolate of tartar wherein, chlorine root≤0.2%, water-insoluble≤0.1%, moisture content≤3%.
3. a kind of method of producing complete water-soluble vitriolate of tartar according to claim 1, wherein Repone K and the sulfuric acid quality percentage composition as raw material is respectively 90-95% Repone K, 98% industrial sulphuric acid.
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| CN2012101201155A CN102633537A (en) | 2012-04-23 | 2012-04-23 | Method for producing watersoluble potassium sulfate |
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| CN2012101201155A CN102633537A (en) | 2012-04-23 | 2012-04-23 | Method for producing watersoluble potassium sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708852A (en) * | 2013-08-12 | 2014-04-09 | 绥芬河市石英经贸有限公司 | Simple-substance high content round hollow granular potassium fertilizer and preparation method thereof |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078226A (en) * | 1993-04-19 | 1993-11-10 | 山东省临沂市化工总厂 | The production method of potassium sulphate type ternary composite fertilizer |
| CN1168874A (en) * | 1997-02-19 | 1997-12-31 | 李守义 | Process for producing compound fertilizer contg. potassium sulfate and ammonium phosphate |
| CN1229777A (en) * | 1999-01-12 | 1999-09-29 | 铜陵化学工业集团公司铜官山化工总厂 | Method for producing sulfonyl nitrogen-potassium compound fertilizer |
| RU2404947C1 (en) * | 2009-04-13 | 2010-11-27 | Тагир Вильданович Шарипов | Method of obtaining complex fertilisers |
-
2012
- 2012-04-23 CN CN2012101201155A patent/CN102633537A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078226A (en) * | 1993-04-19 | 1993-11-10 | 山东省临沂市化工总厂 | The production method of potassium sulphate type ternary composite fertilizer |
| CN1168874A (en) * | 1997-02-19 | 1997-12-31 | 李守义 | Process for producing compound fertilizer contg. potassium sulfate and ammonium phosphate |
| CN1229777A (en) * | 1999-01-12 | 1999-09-29 | 铜陵化学工业集团公司铜官山化工总厂 | Method for producing sulfonyl nitrogen-potassium compound fertilizer |
| RU2404947C1 (en) * | 2009-04-13 | 2010-11-27 | Тагир Вильданович Шарипов | Method of obtaining complex fertilisers |
Non-Patent Citations (1)
| Title |
|---|
| 章永洁: "氯化钾与硫酸转化制取硫酸钾的研究", 《河北工业大学硕士学位论文》, 20 January 2003 (2003-01-20), pages 69 - 6 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708852A (en) * | 2013-08-12 | 2014-04-09 | 绥芬河市石英经贸有限公司 | Simple-substance high content round hollow granular potassium fertilizer and preparation method thereof |
| CN103708852B (en) * | 2013-08-12 | 2016-04-06 | 绥芬河市石英经贸有限公司 | Simple-substance high content round hollow granular potassium fertilizer and preparation method thereof |
| 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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Application publication date: 20120815 |