CN111908488A - High-purity reagent-grade potassium chloride and production method thereof - Google Patents
High-purity reagent-grade potassium chloride and production method thereof Download PDFInfo
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- CN111908488A CN111908488A CN202010747994.9A CN202010747994A CN111908488A CN 111908488 A CN111908488 A CN 111908488A CN 202010747994 A CN202010747994 A CN 202010747994A CN 111908488 A CN111908488 A CN 111908488A
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- potassium chloride
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 142
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 70
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 239000011833 salt mixture Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 10
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 7
- 229910052708 sodium Inorganic materials 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- -1 salt potassium chloride Chemical class 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005185 salting out Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production method of high-purity potassium chloride, belonging to the field of chemical manufacturing. Dissolving industrial-grade potassium chloride at high temperature, and filtering to obtain a crude potassium chloride solution; introducing HCL gas into the crude potassium chloride solution to obtain an acid salt mixed solution; then, carrying out centrifugal treatment and separation on the solution to obtain wet-based high-purity potassium chloride crystals; and baking the crystal at high temperature to obtain the high-purity reagent-grade potassium chloride. The invention utilizes HCL gas to be added into potassium chloride solution to form the same ion effect, and potassium chloride is crystallized and separated out. Compared with other current potassium chloride purification processes, the process can selectively remove sodium ions and heavy metal ions, and is simple, low in operation cost and high in yield of high-purity potassium chloride products of more than 90%.
Description
Technical Field
The invention relates to a production method of high-purity reagent-grade potassium chloride and high-purity reagent-grade potassium chloride prepared by the production method, and belongs to the field of chemical manufacturing.
Background
The reagent grade potassium chloride is colorless, long and thin rhombic or cubic crystal or white crystal powder, has no odor, is salty in taste, is easily soluble in water, is soluble in glycerol and is slightly soluble in ethanol. Along with the improvement of living standard of people, the demand of high-grade refined potassium chloride, especially reagent-grade potassium chloride, is increasing. Sodium ions and heavy metals in industrial potassium chloride have great influence on the quality of products. For example, in the area of the faaida wood of Qinghai province, a large number of salt lakes exist, and particularly, the salt lake brine in the area of Kerr sweat belongs to chloride type brine, so that a large amount of carnallite is produced. When local enterprises adopt a conventional flotation method to produce potassium chloride, a large amount of calcium sulfate is enriched in potassium chloride products, the quality of the potassium chloride products is seriously influenced, and the potassium chloride products cannot reach the lowest level in the national standard. In addition, many industries have special requirements for the content of impurities in high-purity potassium chloride, such as the requirement of the national standard potassium chloride chemical reagent for sodium content index of less than or equal to 0.02 percent, and the requirement of part of special industries even for sodium content index of less than or equal to 0.01 percent
At present, the production process of food-grade potassium chloride at home and abroad is basically an evaporative crystallization process which is used in the last 90 years, and generally comprises the steps of dissolving, removing impurities, crystallizing, filtering and drying.
How to obtain a method for producing high-purity reagent-grade potassium chloride with low sodium and heavy metals, simple method and low cost still needs to be explored and researched urgently in the industry.
Disclosure of Invention
The invention aims to provide a production method of high-purity reagent-grade potassium chloride, which adopts salting-out crystallization to remove impurities to obtain high-purity reagent-grade potassium chloride.
The technical scheme for realizing the purpose is as follows:
a production method of high-purity reagent-grade potassium chloride comprises the steps of dissolving, filtering, salting out, crystallizing, removing impurities, performing centrifugal analysis, and baking at high temperature, and comprises the following specific steps:
(1) dissolving industrial-grade potassium chloride at high temperature, and filtering to obtain a crude potassium chloride solution;
(2) introducing HCL gas into the rough potassium chloride solution to obtain an acid salt mixed solution, and crystallizing and separating out potassium chloride salt;
(3) centrifuging the hydrochloric acid mixture, and separating to obtain wet-based high-purity potassium chloride crystals;
(4) and baking the wet-based potassium chloride at high temperature to obtain the high-purity reagent-grade potassium chloride.
Further, controlling the temperature of the crude potassium chloride solution to be-10-15 ℃ when introducing HCL gas in the step (2).
Further, the content of hydrogen chloride in the acid salt mixed solution in the step (2) is 9% -37%.
Further, in the step (4), the high-temperature baking temperature is 150-300 ℃, and the baking time is 2-8 hours.
The invention also discloses high-purity reagent-grade potassium chloride prepared by any one of the production methods.
Further, the purity of the potassium chloride is more than or equal to 99.6 percent.
The invention has the beneficial effects that:
the invention utilizes HCL gas to be added into potassium chloride solution to form the same ion effect, and potassium chloride is crystallized and separated out. Compared with other current potassium chloride purification processes, the process can selectively remove sodium ions and heavy metal ions, and is simple, low in operation cost and high in yield of high-purity potassium chloride products of more than 90%.
Drawings
FIG. 1 is a flow chart of the production process of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Putting raw salt potassium chloride with the content (weight content) of more than or equal to 90% into a dissolving tank according to the proportion of potassium chloride/pure water =150g/850g, dissolving under a stirring state to obtain a crude potassium chloride salt solution, filtering the solution through a filter, storing the solution in a buffer tank, introducing HCL gas, controlling the temperature of the solution at-10 ℃, stopping introducing when the content of hydrogen chloride in the solution reaches 9%, performing centrifugal separation, introducing the separated potassium chloride into a drying furnace, and drying at 200 ℃ for 2-5h to obtain reagent-grade potassium chloride with the purity of more than or equal to 99.6%, wherein the content of sodium is 0.03%, and the content of iron is 0.3 ppm. Table 1 shows the ion contents after purification.
TABLE 1 ion content of high purity reagent grade potassium chloride obtained in example 1
Example 2
Putting raw salt potassium chloride with the content (weight content) of not less than 90% into a dissolving tank according to the proportion that potassium chloride/pure water =200g/800g, dissolving under a stirring state to obtain a crude potassium chloride salt solution, filtering the solution through a filter, storing the solution in a buffer tank, introducing HCL gas, controlling the temperature of the solution at 15 ℃, stopping introducing when the content of hydrogen chloride in the solution reaches 20%, performing centrifugal separation, introducing the separated potassium chloride into a drying furnace, and drying at 300 ℃ for 2-5h to obtain reagent-grade potassium chloride with the purity of not less than 99.8%, wherein the content of sodium is 0.01% and the content of iron is 0.18 ppm. Table 2 shows the ion contents after purification.
Table 2 ion content of high purity reagent grade potassium chloride obtained in example 2
Example 3
Putting raw salt potassium chloride with the content (weight content) of more than or equal to 90% into a dissolving tank according to the proportion that potassium chloride/pure water =200g/800g, dissolving under a stirring state to obtain a crude potassium chloride salt solution, filtering the solution through a filter, storing the solution in a buffer tank, introducing HCL gas, controlling the temperature of the solution at-5 ℃, stopping introducing when the content of hydrogen chloride in the solution reaches 20%, performing centrifugal separation, introducing the separated potassium chloride into a drying furnace, and drying at 250 ℃ for 2-5h to obtain reagent-grade potassium chloride with the purity of more than or equal to 99.7%, wherein the content of sodium is 0.01% and the content of iron is 0.47 ppm. Table 3 shows the ion contents of the purified potassium chloride.
Table 3 ion content of high purity reagent grade potassium chloride obtained in example 3
According to the regulation of GB/T646-: the pH value passes the test, the iodine and bromine pass the test, the arsenic is less than or equal to 2ppm, the heavy metal is less than or equal to 5ppm, the drying weight loss is less than or equal to 1.0 percent, and the sodium is less than or equal to 0.1 percent. The reagent grade potassium chloride obtained by the invention completely meets the requirements.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (6)
1. A production method of high-purity reagent-grade potassium chloride comprises the following steps:
(1) dissolving industrial-grade potassium chloride at high temperature, and filtering to obtain a crude potassium chloride solution;
(2) introducing HCL gas into the rough potassium chloride solution to obtain an acid salt mixed solution, and crystallizing and separating out potassium chloride salt;
(3) centrifuging the hydrochloric acid mixture, and separating to obtain wet-based high-purity potassium chloride crystals;
(4) and baking the wet-based potassium chloride at high temperature to obtain the high-purity reagent-grade potassium chloride.
2. The production method according to claim 1, wherein the temperature of the crude potassium chloride solution is controlled to be-10 to 15 ℃ when the HCL gas is introduced in the step (2).
3. The production method according to claim 1, wherein the hydrogen chloride content in the acid salt mixture of step (2) is 9% to 37%.
4. The production method according to claim 1, wherein the high-temperature baking temperature in the step (4) is 150 to 300 ℃ and the baking time is 2 to 8 hours.
5. A high purity reagent grade potassium chloride prepared according to any one of the production methods of claims 1 to 4.
6. The high-purity reagent-grade potassium chloride prepared by the production method according to claim 5 is characterized in that the purity of the potassium chloride is more than or equal to 99.6%.
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| CN202010747994.9A CN111908488A (en) | 2020-07-30 | 2020-07-30 | High-purity reagent-grade potassium chloride and production method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910204A (en) * | 2020-07-30 | 2020-11-10 | 华融化学股份有限公司 | Purification process of electronic-grade potassium hydroxide |
| CN115650256A (en) * | 2021-09-26 | 2023-01-31 | 华融化学股份有限公司 | Industrial potassium chloride purification process and production system |
| CN115650280A (en) * | 2022-09-09 | 2023-01-31 | 昆明理工大学 | Preparation method of gallium salt |
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| JP2004149376A (en) * | 2002-10-31 | 2004-05-27 | Tsurumi Soda Co Ltd | Method for producing high purity potassium chloride, apparatus for producing high purity potassium chloride, high purity potassium chloride, and method of using high purity potassium chloride |
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| CN101559958A (en) * | 2009-06-05 | 2009-10-21 | 魏君英 | Method for purifying potassium chloride |
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2020
- 2020-07-30 CN CN202010747994.9A patent/CN111908488A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910204A (en) * | 2020-07-30 | 2020-11-10 | 华融化学股份有限公司 | Purification process of electronic-grade potassium hydroxide |
| CN115650256A (en) * | 2021-09-26 | 2023-01-31 | 华融化学股份有限公司 | Industrial potassium chloride purification process and production system |
| CN115650280A (en) * | 2022-09-09 | 2023-01-31 | 昆明理工大学 | Preparation method of gallium salt |
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