Method for preparing potassium sulfate from brine

A technology of potassium sulfate and brine, which is applied in the preparation of sulfate/bisulfate, tetrafluoroboric acid, boron halide compounds, etc., can solve the problems of high production cost, human health hazards, and high price, and achieve large industrial value and reduce Effects of pollution and resource saving

Inactive Publication Date: 2016-09-28
LIAONING TECHNICAL UNIVERSITY
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  • Abstract
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Problems solved by technology

However, these commonly used precipitants are either toxic and harmful, or expensive or require high reaction conditions during precipitation. For example, dipicrylamine is an explosive and toxic organic solvent, which will cause harm to human health and endanger the environment; perchlorate [1] The price is expensive, the precipitation process must be carried out under low temperature freezing, resulting in high energy consumption, and perchlorate will pollute the environment; gypsum and phosphate [2] The precipitation method requires the use of a large amount of precipitant, resulting in production costs higher than the product value; sodium tetraphenylborate [3] It is a common reagent in analytical chemistry, used for the quantitative detection of potassium ions, rubidium ions, cesium ions, silver ions, thallium ions and ammonium ions. It can form white precipitates with these ions at low temperature, but it is very expensive and cannot be recycled. , will pollute the environment

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  • Method for preparing potassium sulfate from brine

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take brine as the method for preparing potassium sulfate as raw material, the process flow chart is as figure 1 As shown, take 1.5L of the brine described in Table 1, add saturated sodium fluoroborate solution, the molar weight of sodium fluoroborate is 0.476mol, stir and react at room temperature for 20min, filter out the precipitate, and keep the filtrate; Dried and weighed, 52.73gKBF can be obtained 4 solid, the KBF 4 Mix the solid with 21.25g of concentrated sulfuric acid with a mass fraction of 98.3%, heat to 700°C, and collect fluoboric acid gas with a suspension containing 27.0g of sodium bicarbonate, stop the reaction after 50min, dry at 105°C and weigh The solid mass of potassium sulfate was 37.16g, the purity was 98.2%, and the recovery rate of potassium ions was 79.5%.

[0028] Add cetylpyridinium sulfate solution containing 0.0286mol to the filtrate obtained after extracting potassium, immediately generate cetylpyridinium fluoroborate precipitation, filter...

Embodiment 2

[0031] Take brine as the method for preparing potassium sulfate as raw material, the process flow chart is as figure 1 As shown, get 1.5L of brine described in Table 1, add the saturated sodium fluoroborate solution recovered in Example 1, the molar weight of sodium fluoroborate is 0.467mol, after stirring and reacting at room temperature for 20min, filter out the precipitate, and keep the filtrate; The precipitate is dried at 105°C and weighed to obtain 51.78gKBF 4 solid, the KBF 4 Mix the solid with 21.05g of concentrated sulfuric acid with a mass fraction of 98.3%, heat to 700°C, and collect fluoboric acid gas with a suspension containing 25.0g of sodium bicarbonate, stop the reaction after 50min, dry at 105°C and weigh The solid mass of potassium sulfate is 36.45g, the purity is 98.3%, and the recovery rate of potassium ions is 78.1%.

[0032]Add the solution containing 0.0282mol cetylpyridinium sulfate recovered in embodiment 1 to the filtrate obtained after extracting ...

Embodiment 3

[0035] Take brine as the method for preparing potassium sulfate as raw material, the process flow chart is as figure 1 As shown, take 1L of the brine described in Table 1, add saturated ammonium fluoroborate solution, the molar weight of ammonium fluoroborate is 0.380mol, stir and react at room temperature for 20min, filter out the precipitate, and keep the filtrate; dry the precipitate at 105°C , weighing, 39.54gKBF can be obtained 4 solid, the KBF 4 The solid is mixed with 15.94g of concentrated sulfuric acid with a mass fraction of 98.3%, heated to 600°C, and the fluoroboric acid gas is collected with a solution containing 30.0g of ammonium bicarbonate. After 90 minutes, the reaction is stopped, and potassium sulfate is weighed after drying at 105°C. The solid mass was 28.15g, the purity was 97.2%, and the recovery rate of potassium ions was 89.4%.

[0036] Add dodecyltrimethylammonium sulfate solution to the filtrate obtained after extracting potassium, immediately gener...

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Abstract

The invention discloses a method for preparing potassium sulfate from brine. The method comprises that a borofluoride is added into brine, the mixture undergoes a reaction at the room temperature, the reaction product is filtered so that potassium borofluoride solids are obtained, the filtrate is collected, the potassium borofluoride solids and concentrated sulfuric acid directly undergo a reaction to produce potassium sulfate solids and fluoroboric acid gas, water-soluble quaternary ammonium sulfate is added into the filtrate so that fluoborate ions in the filtrate are transformed into quaternary ammonium cationic borofluoride, the quaternary ammonium cationic borofluoride further reacts with concentrated sulfuric acid to produce fluoroboric acid gas and a water-soluble quaternary ammonium sulfate solution to be recovered, the fluoroboric acid gas obtained by the two steps are respectively absorbed by an absorbent so that the fluoroboric acid gas is transformed into a borofluoride, the reaction solution is concentrated until saturation and the saturated reaction solution is recovered and then is used in a reaction of a borofluoride and brine. The method mainly comprises two steps, has a fast reaction rate and a high conversion rate, has a potassium ion recovery rate of 92% or more, produces a potassium sulfate product with purity of 97-99% and can be directly applied for crops.

Description

technical field [0001] The invention relates to a method for preparing potassium sulfate in the field of inorganic chemical industry, in particular to a method for preparing potassium sulfate by using brine as a raw material. Background technique [0002] Potassium sulfate is an important chlorine-free high-quality potassium fertilizer. It has a low saline-alkali soil index, is suitable for a wide range of crops, and can provide sulfur trace elements. It can not only increase crop yield, but also improve crop quality. However, my country is a country that is relatively deficient in potassium resources, and a large amount of potassium fertilizers are dependent on imports. Therefore, the method for preparing potassium sulfate at a lower cost by using easy-to-obtain raw materials has become a hot spot of current research. [0003] Brine is a kind of water with strong mineralization, including salt lake brine, underground brine, sea salt brine, etc., which contains a lot of mag...

Claims

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Application Information

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IPC IPC(8): C01D5/02C01B35/06
CPCC01B35/063C01B35/066C01D5/02C01P2006/80
Inventor 张树东武振闫平科张旭
Owner LIAONING TECHNICAL UNIVERSITY
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