CN1150121A - Salting out process for producing potassium sulfate - Google Patents

Salting out process for producing potassium sulfate Download PDF

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Publication number
CN1150121A
CN1150121A CN 96109835 CN96109835A CN1150121A CN 1150121 A CN1150121 A CN 1150121A CN 96109835 CN96109835 CN 96109835 CN 96109835 A CN96109835 A CN 96109835A CN 1150121 A CN1150121 A CN 1150121A
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CN
China
Prior art keywords
potassium
potassium sulfate
sulfate
chloride
sulfuric acid
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Pending
Application number
CN 96109835
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Chinese (zh)
Inventor
殷洪
龙文杰
冯玉梅
杨国强
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Qinghua Ziguang (group) General Co
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Qinghua Ziguang (group) General Co
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Publication date
Application filed by Qinghua Ziguang (group) General Co filed Critical Qinghua Ziguang (group) General Co
Priority to CN 96109835 priority Critical patent/CN1150121A/en
Publication of CN1150121A publication Critical patent/CN1150121A/en
Pending legal-status Critical Current

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Abstract

A salting-out process for preparing potassium sulfate from sulfuric acid, potassium chloride and ammonia includes such steps as low-temp reaction of potassium chloride on sulfuric acid to generate potassium hydrogen sulfate, addition of potassium chloride to prepare its aqueous solution, low-temp. neutralization with ammonia to generate potassium sulfate and ammonium chloride and water washing to separate potassium sulfate. Its advantages are high transform rate of K and quality of product, low corrosion to apparatus, and low technological temp., energy consumption and cost.

Description

Process for preparing potassium sulfate by salting-out method
The present invention relates to a production process of potassium sulfate, belonging to the field of inorganic chemical technology.
The production of potassium sulfate by using potassium chloride and sulfuric acid as raw materials is a main method for industrial production of potassium sulfate. At present, five methods are mainly used at home and abroad to convert potassium chloride, namely a dry heating method, an association method, a solvent extraction method, a neutralization synthesis method, a liquid phase conversion method and a neutral one-step method. The representative dry heat method is Mannheim furnace method, which comprises mixing potassium chloride and sulfuric acid at relatively low temperature to obtain potassium bisulfate, heating to 500-700 deg.C in Mannheim furnace, and reacting to obtain potassium sulfate. The method has the disadvantages of high reaction temperature, high energy consumption, serious corrosion and frequent equipment replacement; the association method utilizes the property of different affinity of association agent to hydrochloric acid and sulfuric acid to obtain potassium sulfate with higher purity. The method has the disadvantages of low equipment utilization rate, large occupied area and high consumption of the association agent; the solvent extraction method is divided into a post-extraction hydrochloric acid method and a pre-association sulfuric acid method. The method has the disadvantages of more operation steps, complicated regeneration of post-extraction or association agent, large loss in the whole process and high production cost; the neutralization synthesis method is characterized by that it utilizes two-step reaction at lower temp., and its by-products are hydrochloric acid and ammonium sulfate. The method has the disadvantages of small yield per unit and large evaporation capacity; the liquid phase conversion method, which is a one-step reaction to generate potassium sulfate, has the disadvantages of large solid-liquid circulation amount, long process flow, low yield and difficult large-scale production; the neutral one-step process for producing potassium sulfate with sulfuric acid, ammonium hydrogen chloride and potassium chloride as raw materials has the disadvantages of long reaction time, harsh operation conditions and high production cost.
The invention aims to provide a production process for preparing potassium sulfate by usingsulfuric acid, potassium chloride and ammonia as raw materials at a lower temperature.
The potassium sulfate producing process includes the reaction of potassium chloride and sulfuric acid as material at low temperature to produce potassium bisulfate, the addition of potassium chloride to produce water solution, the neutralization of the water solution with ammonia at low temperature to produce potassium sulfate and ammonium chloride, and the water washing to separate. Namely, the method is to generate and separate potassium sulfate products by utilizing the principle that the solubility of potassium sulfate and ammonium chloride in an alkaline solution is greatly different.
The specific process comprises the following steps:
1. preparation of potassium hydrogen sulfate
Mixing potassium chloride and sulfuric acid according to the mol ratio of 1: 0.4-1.8, heating to gradually raise the temperature to 30-180 ℃, and continuously reacting under the condition of stirring until hydrogen chloride is completely escaped, wherein the reaction formula is as follows:
2. formation of potassium sulfate
Adding the generated potassium bisulfate and potassium chloride into a reactor according to the molar ratio of the potassium bisulfate to the potassium chloride of 1: 0.5-1.5, adding a proper amount of water for dissolving, introducing ammonia for neutralizing, and keeping the pH value of the solution within the range of 7.0-14 to generate potassium sulfate and ammonium chloride. The reaction formula is as follows:
washing with water, filtering and separating potassium sulfate to obtain agricultural orindustrial potassium sulfate product, with the total amount of water being 0.5-5 times of the solid amount and the washing times being 1-3 times.
Illustrative examples are as follows:
the process is carried out by using 500 g of 98% sulfuric acid or 526.9 g of 93% sulfuric acid (490 g of 100% sulfuric acid), 778.9 g of 95% potassium chloride (740 g of potassium chloride), 257.8 g of 24% ammonia water (61.87 g of 100% ammonia), and obtaining 826.5 g of potassium sulfate, 529.8 g of 31% hydrochloric acid, 254.5 g of ammonium chloride, 98% over potassium recovery rate, 90% hydrochloric acid recovery rate, 98.8% sulfuric acid utilization rate and 95% ammonia utilization rate. The quality of the obtained product is as follows:
content of name free acid content chlorine content
96.25 percent to 1.0 percent of potassium sulfate
Hydrochloric acid 31%/_ X
99.3% ammonium chloride/none
The present invention adopts salting-out process, and has complete and fast reaction, simple technological process, low cost, low temperature, low power consumption, less corrosion to apparatus, long service life of apparatus, closed circulation and no three waste exhaust. The conversion rate of potassium is more than 98%, and the obtained product has low chlorine content, high purity and good quality. Is suitable for the industrial production of potassium sulfate with different specifications.

Claims (4)

1. A process for preparing potassium sulfate from sulfuric acid and potassium chloride includes such steps as reaction between potassium chloride and sulfuric acid at lowtemp (30-180 deg.C) to obtain potassium hydrogen sulfate, adding potassium chloride to obtain aqueous solution, adding ammonia at low temp (30-180 deg.C) to neutralize until the solution is alkaline, generating potassium sulfate and ammonium chloride, and washing with water.
2. The process for producing potassium sulfate as claimed in claim 1, wherein the molar ratio of potassium chloride to sulfuric acid is 1: 0.4-1.8.
3. The process for producing potassium sulfate as claimed in claim 1, wherein the molar ratio of potassium bisulfate to potassium chloride is 1: 0.5-1.5.
4. The process for producing potassium sulfate as claimed in claim 1, wherein the amount of ammonia added is such that the pH of the reaction solution is in the range of 7.0 to 14.
CN 96109835 1996-09-20 1996-09-20 Salting out process for producing potassium sulfate Pending CN1150121A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 96109835 CN1150121A (en) 1996-09-20 1996-09-20 Salting out process for producing potassium sulfate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 96109835 CN1150121A (en) 1996-09-20 1996-09-20 Salting out process for producing potassium sulfate

Publications (1)

Publication Number Publication Date
CN1150121A true CN1150121A (en) 1997-05-21

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ID=5120649

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 96109835 Pending CN1150121A (en) 1996-09-20 1996-09-20 Salting out process for producing potassium sulfate

Country Status (1)

Country Link
CN (1) CN1150121A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236448A (en) * 2015-10-14 2016-01-13 四川蓥峰实业有限公司 New process for production of potassium sulfate and co-production of compound fertilizer
CN106382988A (en) * 2015-12-01 2017-02-08 中国科学院上海技术物理研究所 Hyper-spectral imager based on step optical filter

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236448A (en) * 2015-10-14 2016-01-13 四川蓥峰实业有限公司 New process for production of potassium sulfate and co-production of compound fertilizer
CN105236448B (en) * 2015-10-14 2017-07-04 四川蓥峰实业有限公司 A kind of new technology for producing coproduction of potassium sulfate composite fertilizer
CN106382988A (en) * 2015-12-01 2017-02-08 中国科学院上海技术物理研究所 Hyper-spectral imager based on step optical filter

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