CN113666389B - Preparation method of decolored potassium chloride solution - Google Patents
Preparation method of decolored potassium chloride solution Download PDFInfo
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- CN113666389B CN113666389B CN202010403263.2A CN202010403263A CN113666389B CN 113666389 B CN113666389 B CN 113666389B CN 202010403263 A CN202010403263 A CN 202010403263A CN 113666389 B CN113666389 B CN 113666389B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/36—Reactivation or regeneration
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/16—Purification by precipitation or adsorption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/18—Purification with selective solvents
Abstract
In order to solve the problem of poor decolorizing effect of potassium chloride solution in the prior art, the invention provides a preparation method of the decolorizing potassium chloride solution, which comprises the following operation steps: heating the potassium chloride slag raw material to obtain a potassium chloride slag intermediate, dissolving the potassium chloride slag intermediate in a solvent to obtain a potassium chloride solution, adding an oxidant and an adsorbent into the potassium chloride solution, and separating the adsorbent to obtain a decolored potassium chloride solution, wherein the adsorbent comprises activated carbon and polyacrylamide, and the activated carbon is activated by nitric acid. In the preparation method of the decolored potassium chloride solution, the decoloration performance is good, the production process and the use are simple and convenient, the decoloration effect is stable, and the preparation method is suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of reutilization of waste salt resources, and particularly relates to a preparation method of a decolored potassium chloride solution.
Background
Potassium chloride is a versatile inorganic salt. Potassium chloride is mainly used in the inorganic industry and is a basic raw material for producing various potassium salts or bases such as potassium hydroxide, potassium sulfate, potassium nitrate, potassium chlorate, potassium bichromate and the like. The medicine industry is used as diuretic and medicine for preventing and curing potassium deficiency.
In some organic or inorganic chemical production processes, potassium chloride waste salt is often generated, the potassium chloride waste salt contains a large amount of organic or inorganic impurities, cannot be directly used as industrial raw material salt, and constitutes a great threat to the environment, the salt and the impurities are extremely easy to run off, the surrounding soil is salinized, the surrounding vegetation is endangered, and meanwhile, the pollution is caused to surrounding rivers, water sources, paddy fields and the like. So the potassium chloride with higher purity can be obtained only by removing impurities, oxidizing and decoloring the waste potassium chloride.
The prior decoloring technology for treating the potassium chloride waste salt mainly comprises the following steps: adsorption decolorization, coagulation decolorization, oxidation decolorization, electrolytic decolorization, biological decolorization, flocculation decolorization, etc. However, the components of the potassium chloride solution are complex and changeable, only one decoloring technology cannot meet the decoloring treatment requirement of the potassium chloride solution, and how to improve the decoloring and impurity removing effects of the potassium chloride waste salt is a problem to be solved in the field.
Disclosure of Invention
Aiming at the problem of poor decoloring effect of the potassium chloride solution in the prior art, the invention provides a preparation method of the decoloring potassium chloride solution.
The technical scheme adopted by the invention for solving the problems is as follows:
the invention provides a preparation method of a decolored potassium chloride solution, which comprises the following operation steps:
heating the potassium chloride slag raw material to obtain a potassium chloride slag intermediate;
dissolving the potassium chloride salt slag intermediate in a solvent to obtain a potassium chloride solution;
adding an oxidant to the potassium chloride solution;
adding an adsorbent into the potassium chloride solution, and separating the adsorbent to obtain a decolorized potassium chloride solution;
the adsorbent comprises activated carbon and polyacrylamide, and the activated carbon is activated by nitric acid.
Optionally, in the adsorbent, the mass ratio of the activated carbon to the polyacrylamide is (9.5-9.9) (0.1-0.5).
Optionally, the nitric acid activation treatment comprises:
controlling the pH value of nitric acid to be less than 3, and completely immersing the activated carbon in the nitric acid;
separating the activated carbon from the nitric acid, spraying the activated carbon, and drying to obtain the nitric acid activated carbon.
Optionally, before or simultaneously with the heating treatment, adding an alkaline auxiliary agent into the potassium chloride salt slag raw material, wherein the mass ratio of the potassium chloride salt slag raw material to the alkaline auxiliary agent is (9.0-9.5) (0.5-1.0).
Optionally, the alkaline auxiliary comprises KOH and Ca (OH) 2 One or two of them.
Optionally, the temperature of the heating treatment is 120-200 ℃.
Optionally, the solvent is selected from water, and the mass ratio of the solvent to the potassium chloride salt slag intermediate is 2:1-4:1.
Optionally, the oxidant comprises hydrogen peroxide and/or sodium hypochlorite, and the addition amount of the oxidant is 2% -8% based on 100% of the total mass of the potassium chloride solution.
Optionally, the adsorbent is added in an amount of 1% -3% based on 100% of the total mass of the potassium chloride solution.
Optionally, the potassium chloride salt slag raw material comprises potassium chloride, carbon-containing organic matters and potassium fluoride.
Optionally, before the "adding an adsorbent to the potassium chloride solution", further comprising:
adding a calcium salt to the potassium chloride solution.
The invention adopts polyacrylamide and nitric acid activated carbon as adsorbents to treat potassium chloride solution, and the inventor surprisingly finds that the polyacrylamide and the nitric acid activated carbon have obvious synergistic effect, compared with a single component, the adsorbents formed by compounding two substances can show more excellent adsorption performance under the condition of the same additive amount, so that the removal efficiency of organic pigment and other impurities in the potassium chloride solution can be improved, and the use amount of the adsorbents can be reduced, thereby ensuring that the invention has good decolorization performance, reduces the production process cost, is simple and convenient to use, has stable decolorization effect and is suitable for large-scale production.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the invention more clear, the invention is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a preparation method of a decolored potassium chloride solution, which comprises the following operation steps:
heating the potassium chloride slag raw material to obtain a potassium chloride slag intermediate;
dissolving the potassium chloride salt slag intermediate in a solvent to obtain a potassium chloride solution;
adding an oxidant to the potassium chloride solution;
adding an adsorbent into the potassium chloride solution, and separating the adsorbent to obtain a decolorized potassium chloride solution;
the adsorbent comprises activated carbon and polyacrylamide, and the activated carbon is activated by nitric acid.
The invention adopts polyacrylamide and nitric acid activated carbon as adsorbents to treat potassium chloride solution, and the inventor surprisingly finds that the polyacrylamide and the nitric acid activated carbon have obvious synergistic effect, compared with a single component, the adsorbents formed by compounding two substances can show more excellent adsorption performance under the condition of the same additive amount, so that the removal efficiency of organic pigment and other impurities in the potassium chloride solution can be improved, and the use amount of the adsorbents can be reduced, thereby ensuring that the invention has good decolorization performance, reduces the production process cost, is simple and convenient to use, has stable decolorization effect and is suitable for large-scale production.
The activated carbon is activated with nitric acid to increase the specific surface area of the activated carbon, thereby increasing the adsorption effect.
In some embodiments of the invention, the mass ratio of the activated carbon to the polyacrylamide in the adsorbent is (9.5-9.9): 0.1-0.5.
Compared with the single adsorbent, the activated carbon activated by nitric acid and polyacrylamide have better adsorption and decolorization effects, have stronger flocculation, adhesion and trapping effects on fine particle impurities in the potassium chloride solution, and have lower combined use amount and clearer solution. If the ratio of polyacrylamide in the adsorbent is too high, the potassium chloride solution is too viscous, and the generated waste residue is too much, which in turn deteriorates the decoloring effect of the present invention. In the adsorbent, if the ratio of the activated carbon is too high, namely the usage amount of polyacrylamide is too small, the decoloring effect of the invention is not obvious.
In some embodiments of the invention, the nitric acid activation process comprises:
controlling the pH value of nitric acid to be less than 3, and completely immersing the activated carbon in the nitric acid;
separating the activated carbon from the nitric acid, spraying the activated carbon, and drying to obtain the nitric acid activated carbon.
More preferably, the pH value of nitric acid is controlled to be less than 3, the activated carbon is fully immersed in the nitric acid, and the mixture is stirred for 1h at 75-85 ℃;
and (3) cooling, centrifugally separating the activated carbon and the nitric acid, spraying the activated carbon with pure water, and drying to obtain the activated carbon activated by the nitric acid.
The activated carbon with larger specific surface area and more uniform pore size distribution is obtained by controlling the pH value of nitric acid, preserving heat, stirring, cooling, centrifuging and spraying to clean the activated carbon.
In some embodiments of the invention, an alkaline auxiliary agent is added to the potassium chloride salt slag raw material before or simultaneously with the heat treatment, wherein the mass ratio of the potassium chloride salt slag raw material to the alkaline auxiliary agent is (9.0-9.5) (0.5-1.0).
In the invention, organic matters with chromaticity contained in the potassium chloride slag raw material are distilled out or carbonized and polymerized by using a heating treatment method, and the alkali auxiliary agent is used, so that carbonization and decomposition of carbon-containing organic matters such as carbonate polymers and the like can be promoted, the removal efficiency of the carbon-containing organic matters in subsequent operation is improved, and the obtaining of the potassium chloride slag intermediate is quickened.
In some embodiments of the invention, the alkaline promoter comprises KOH and Ca (OH) 2 One or two of them.
In a preferred embodiment, the alkaline promoter is selected from potassium hydroxide, which is advantageous in avoiding the introduction of impurity elements in subsequent operations.
In some embodiments of the invention, the temperature of the heat treatment is 120-200 ℃.
If the temperature of the heating treatment is more than 200 ℃, a large amount of heat and gas can be generated, and the safety of experimental equipment is threatened. The temperature of the heating treatment is lower than 120 ℃, and the effect of decomposing impurity organic matters in the potassium chloride salt slag raw material by the heating treatment is not obvious.
More preferably, the temperature of the heat treatment is controlled in the range of 150 to 160 ℃.
In some embodiments of the invention, the solvent is selected from water, and the mass ratio of the solvent to the potassium chloride salt slag intermediate is 2:1-4:1.
More preferably, the mass ratio of the solvent to the potassium chloride salt slag intermediate is 3:1-4:1.
In some embodiments of the present invention, the oxidizing agent comprises hydrogen peroxide and/or sodium hypochlorite, and the amount of the oxidizing agent added is 2% -8% based on 100% of the total mass of the potassium chloride solution.
More preferably, the addition amount of the oxidizing agent is 2% to 5% based on 100% of the total mass of the potassium chloride solution.
Hydrogen peroxide or sodium hypochlorite is used as the oxidant, and hydrogen peroxide and sodium hypochlorite are stronger oxidants, so that organic matters due to carbonization and decomposition and carbonization and polymerization can be oxidized and treated, and the decoloring effect is improved.
In some embodiments of the invention, the adsorbent is added in an amount of 1% to 3% based on 100% of the total mass of the potassium chloride solution.
More preferably, the adsorbent is added in an amount of 1% to 3% based on 100% of the total mass of the potassium chloride solution.
In some embodiments of the invention, the potassium chloride salt slag feedstock comprises potassium chloride, carbon-containing organics, and potassium fluoride.
The carbon-containing organic matter comprises a carbonate polymer.
Because fluoride ions are included in the potassium chloride slag raw material, the method further comprises the following steps before the step of adding the adsorbent into the potassium chloride solution:
and adding calcium salt into the potassium chloride solution, and combining and precipitating fluoride ions and calcium ions. The precipitate formed can be separated in a subsequent operation of separating the adsorbent, thereby effectively reducing impurity ions in the potassium chloride solution.
In some embodiments of the invention, the potassium chloride salt residue intermediate is dissolved in a solvent, an oxidizing agent is added to the potassium chloride solution, and an adsorbent is added to the potassium chloride solution, and the adsorbent is removed by stirring and filtering, wherein the stirring time is 1-4 hours.
More preferably, the stirring time is 1 to 2 hours.
The invention is further illustrated by the following examples. It is to be understood that the present invention is not limited to the following embodiments, and the methods are regarded as conventional methods unless otherwise specified. Materials are commercially available from public sources unless otherwise indicated.
Example 1
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 150 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the potassium chloride salt slag intermediate in the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, wherein the decolorized potassium chloride solution is marked as S1.
Example 2
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Sodium hypochlorite 50g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 150 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding sodium hypochlorite according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S2.
Example 3
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 160 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S3.
Example 4
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 20g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 150 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S4.
Example 5
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 20g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 150 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S5.
Example 6
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 20g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, the potassium chloride slag raw material is put into a muffle furnace to be baked for 24 hours at 150 ℃ and then taken out, so as to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 2 hours;
(4) Adding the adsorbent according to the components, stirring for 2 hours, and filtering to obtain a decolored potassium chloride solution, and marking as S6.
Example 7
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) Potassium hydroxide 10g
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) Adding potassium hydroxide into the potassium chloride slag raw materials according to the components, mixing, placing the mixture in a muffle furnace, setting 150 ℃ and baking for 24 hours, and taking out to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the potassium chloride salt slag intermediate in the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S7.
Example 8
This example is intended to illustrate the preparation of the decolorized potassium chloride solution disclosed herein.
The preparation method of the potassium chloride solution comprises the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 20g of anhydrous calcium chloride
(3) 800g of tap water
(4) Hydrogen peroxide 50g
(5) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, and the activated carbon is activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, placing the potassium chloride slag raw material into a muffle furnace, setting 150 ℃ and baking for 24 hours, and taking out to obtain a potassium chloride slag intermediate;
(2) Adding tap water into the potassium chloride salt slag intermediate in the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding calcium chloride into the potassium chloride solution, and stirring for 1h;
(4) Adding hydrogen peroxide according to the components, and stirring for 1h;
(5) Adding the adsorbent according to the components, stirring for 1h, and filtering to obtain decolorized potassium chloride solution, and marking as S8.
Comparative example 1
This example is a comparative illustration of the preparation of the decolorized potassium chloride solution disclosed herein.
The comparative preparation of the potassium chloride solution included the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (powdered activated carbon, activated carbon activated with nitric acid)
The preparation method comprises the following steps:
(1) According to the components, taking a potassium chloride salt slag raw material, setting 150 ℃ in a muffle furnace, baking for 24 hours, and taking out to obtain a potassium chloride salt slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) The above components are added with the adsorbent, stirred for 1h, and filtered to obtain a comparative potassium chloride solution, labeled D1.
Comparative example 2
This example is a comparative illustration of the preparation of the decolorized potassium chloride solution disclosed herein.
The comparative preparation of the potassium chloride solution included the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (polyacrylamide)
The preparation method comprises the following steps:
(1) According to the components, taking a potassium chloride salt slag raw material, setting 150 ℃ in a muffle furnace, baking for 24 hours, and taking out to obtain a potassium chloride salt slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) The above components are added with the adsorbent, stirred for 1h, and filtered to obtain a comparative potassium chloride solution, labeled as D2.
Comparative example 3
This example is a comparative illustration of the preparation of the decolorized potassium chloride solution disclosed herein.
The comparative preparation of the potassium chloride solution included the following material components:
(1) 200g of potassium chloride salt slag raw material
(2) 800g of tap water
(3) Hydrogen peroxide 50g
(4) 10g of adsorbent (the adsorbent comprises powdered activated carbon and polyacrylamide powder, the activated carbon is not activated by nitric acid)
The preparation method comprises the following steps:
(1) According to the components, taking a potassium chloride salt slag raw material, setting 150 ℃ in a muffle furnace, baking for 24 hours, and taking out to obtain a potassium chloride salt slag intermediate;
(2) Adding tap water into the step (1) according to the components to obtain a black turbid potassium chloride solution, and stirring until the black turbid potassium chloride solution is fully dissolved;
(3) Adding hydrogen peroxide according to the components, and stirring for 1h;
(4) The above components are added with the adsorbent, stirred for 1h, and filtered to obtain a comparative potassium chloride solution, labeled as D3.
Evaluation of Performance
Colorimetric test
And respectively taking potassium chloride solutions S1-S8 and comparative potassium chloride solutions D1-D3 to carry out color comparison with a standard sample colorimetric tube, and detecting the fluorine ion content in the potassium chloride solution by adopting a chemical titration method.
The results of the test are shown in table 1.
TABLE 1
| Numbering device | Chromaticity (Hazen) | Fluoride ion content (mg/L) |
| S1 | Light transparent (30-35) | 1500 |
| S2 | Pale yellow transparent (45-50) | 1460 |
| S3 | Light transparent (20-25) | 1490 |
| S4 | Pale yellow transparent (45-50) | 1530 |
| S5 | Light transparent (20-25) | 1520 |
| S6 | Light transparent (20-25) | 1410 |
| S7 | Light transparent (15-20) | 1470 |
| S8 | Light transparent (30-35) | 0.15 |
| D1 | Yellow turbidity (155-160) | 1505 |
| D2 | Black and red | 1450 |
| D3 | Deep yellow transparent (250-255) | 1490 |
As is clear from Table 1, the potassium chloride solutions obtained in examples S1 to S8 were higher in transparency than those obtained in comparative examples D1 to D3, indicating that the activated carbon activated by the polyacrylamide-nitric acid complex as an adsorbent was better in decoloring effect and was able to remove pigments or other organic impurities from the potassium chloride solution more effectively.
The test results of comparative example 7 and example 1 show that the addition of the alkaline auxiliary agent during the heat treatment can effectively promote the decomposition of the organic impurities in the potassium chloride slag raw material, thereby reducing the impurity content in the decolored potassium chloride solution.
The test results of comparative example 8 and example 1 show that the addition of calcium salt to the potassium chloride solution can promote the precipitation of fluoride ions therein, effectively reducing the impurity ion content in the potassium chloride solution.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The preparation method of the decolored potassium chloride solution is characterized by comprising the following operation steps:
heating the potassium chloride slag raw material to obtain a potassium chloride slag intermediate; before or while heating treatment, adding an alkaline auxiliary agent into the potassium chloride salt slag raw material;
dissolving the potassium chloride salt slag intermediate in a solvent to obtain a potassium chloride solution;
adding an oxidant to the potassium chloride solution;
adding an adsorbent into the potassium chloride solution, and separating the adsorbent to obtain a decolorized potassium chloride solution;
the adsorbent comprises active carbon and polyacrylamide, wherein the active carbon is activated by nitric acid, and the mass ratio of the active carbon to the polyacrylamide in the adsorbent is (9.5-9.9) (0.1-0.5).
2. The method for producing a decolorized potassium chloride solution according to claim 1, wherein said nitric acid activation treatment comprises:
controlling the pH value of nitric acid to be less than 3, and completely immersing the activated carbon in the nitric acid;
separating the activated carbon from the nitric acid, spraying the activated carbon, and drying to obtain the nitric acid activated carbon.
3. The method for preparing decolorized potassium chloride solution according to claim 1, wherein the mass ratio of the potassium chloride salt residue raw material to the alkaline auxiliary agent is (9.0-9.5): 0.5-1.0;
the alkaline auxiliary agent comprises KOH and Ca (OH) 2 One or two of them.
4. The method for producing a decolorized potassium chloride solution according to claim 1, wherein the temperature of the heat treatment is 120 to 200 ℃.
5. The method for preparing a decolorized potassium chloride solution according to claim 1, wherein the solvent is selected from water, and the mass ratio of the solvent to the potassium chloride salt residue intermediate is 2:1 to 4:1.
6. The method for preparing decolorized potassium chloride solution according to claim 1, wherein the oxidizing agent comprises hydrogen peroxide and/or sodium hypochlorite, and the addition amount of the oxidizing agent is 2% -8% based on 100% of the total mass of the potassium chloride solution.
7. The method for producing a decolorized potassium chloride solution according to claim 1, wherein the adsorbent is added in an amount of 1 to 3% based on 100% by mass of the total potassium chloride solution.
8. The method for preparing a decolorized potassium chloride solution according to claim 1, wherein the potassium chloride salt residue raw material comprises potassium chloride, carbon-containing organic matters and potassium fluoride.
9. The method for producing a decolorized potassium chloride solution according to claim 8, further comprising, before "adding an adsorbent to the potassium chloride solution:
adding a calcium salt to the potassium chloride solution.
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