CN106495189A - A kind of production method of high-purity food-grade potassium chloride - Google Patents
A kind of production method of high-purity food-grade potassium chloride Download PDFInfo
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- CN106495189A CN106495189A CN201611064836.3A CN201611064836A CN106495189A CN 106495189 A CN106495189 A CN 106495189A CN 201611064836 A CN201611064836 A CN 201611064836A CN 106495189 A CN106495189 A CN 106495189A
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- potassium chloride
- exchange resin
- food
- grade
- ion exchange
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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
- C01D3/145—Purification by solid ion-exchangers or solid chelating agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/04—Halides
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- 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 kind of production method of high-purity food-grade potassium chloride, including dissolving, filtration, ion exchange resin adsorption and purification, condensing crystallizing, centrifugation, drying process, the method for obtaining food-class high-purity potassium chloride after ion exchange resin adsorption-edulcoration.The present invention produces food-grade potassium chloride by ion exchange resin adsorption and purification, purified industrial potassium chloride.Ion exchange resin treatment ability is big, can optionally remove sodium ion and heavy metal ion, renewable use, and long working life, operating cost are relatively low.The technological process of the present invention is simple, can obtain that particle is big and uniform high-grade potassium chloride.
Description
Technical field
The present invention relates to a kind of production method of high-purity food-grade potassium chloride, belongs to chemical industry manufacture field.
Background technology
Food-grade potassium chloride, is colourless elongated rhombus or cubic crystal or white crystalline powder, and odorless, taste are salty, be soluble in
Water, it is dissolved in glycerine, is slightly soluble in ethanol.With the improvement of people's living standards, for high-grade refined potassium chloride, particularly food
The needs of level and medical grade potassium chloride are increasing.In industrial potassium chloride, sodium ion and heavy metal produce very big shadow to product quality
Ring.Such as, there is large number of salt lake in Qinghai Province Qaidam area, especially Cha Er Han area salt lake bittern belongs to chlorination
Thing type bittern, produces a large amount of carnallites.When domestic enterprise produces potassium chloride using conventional flotation method, calcium sulfate can be enriched with a large number
In Potassium Chloride Product, Potassium Chloride Product quality is had a strong impact on so that Potassium Chloride Product is unable to reach most low in national standard
Level.Additionally, the impurity content during much industries are to high purity potassium chloride has particular/special requirement, such as national standard《Chemical reagent potassium chloride》
In require that sodium content index≤0.02%, part special industry even require sodium content index≤0.01%.
The production technology of production food-grade potassium chloride substantially continues to use the evaporation knot of the nineties in last century both at home and abroad at present
Brilliant technique, its technique generally comprise dissolving, removal of impurities, crystallization, filtration and drying.Removal of impurities typically adopts multistage method for crystallising, this
Although method can produce the potassium chloride for conforming to quality requirements, production cost is high, and energy resource consumption is high, it is impossible to which continuous prodution is led
Cause yields poorly, and potassium chloride crystalline particle is little and uneven, easily lumps hardened.Though there are many patents to update evaporative crystallization stream
Journey and device so that the energy consumption of production potassium chloride decreases, and improves to some extent, but technological process is more multiple in product quality
Miscellaneous, some add chemical anticaking agent to prevent product caking, cause products application to be restricted.
CN 105668592A disclose a kind of production method of low sodium high-purity potassium chloride, be strictly control mother liquor in calcium,
The content of the foreign ions such as magnesium and sodium, is continuously replenished fresh saturated potassium chloride solution, this method technique in crystallization
Flow process is complicated, the yielding poorly of product, high cost, while can not be well by foreign ion control in certain scope, product
Quality is unstable, and effect is general.CN 105060315A disclose the side that a kind of employing absorbing process produces food-grade potassium chloride
Method, including works such as dissolving, filtration, multistage macroporous resin adsorption purifying, charcoal absorption, condensing crystallizing, separation of solid and liquid, dryings
Sequence, is purified by macroporous resin adsorption, combines octadecylamine, dodecyl beautiful jade and 2# that activated carbon is removed in industrial potassium chloride
Oil, and for the heavy metals such as sodium ion, magnesium, calcium ion are removed, be then by adding novel substance to system, forming mistake after precipitation
Filter, this simple process can not be such that Potassium Chloride Product sodium ion and heavy metal ion content controls in relatively low scope, not only
The requirement of edible potassium chloride can not be met, and for removing the novel substance that impurity is added, make whole technological process complicated, cost increases
Plus.Therefore, in the production high-grade Process of Potassium Chloride such as food-grade and pharmaceutical grade, production cost, improve product quality how are reduced
It is still the key issue that urgent need is solved with stability.
Content of the invention
It is an object of the invention to provide a kind of production method of high-purity food-grade potassium chloride, is entered using ion exchange resin
Row removal of impurities, obtains highly purified food-grade potassium chloride.
Realize that the technical scheme of above-mentioned purpose is as follows：
A kind of production method of high-purity food-grade potassium chloride, including dissolving, filtration, ion exchange resin adsorption and purification, dense
Sheepshank crystalline substance, centrifugation, drying process, comprise the following steps that：
(1) dissolve：Under room temperature, by potassium chloride raw material stirring and dissolving；
(2) filter：Klorvess Liquid is filtered, sediment is removed；
(3) ion exchange resin adsorption and purification：Klorvess Liquid is pumped into ion exchange resin column to be adsorbed；
(4) condensing crystallizing：Klorvess Liquid after by absorption carries out condensing crystallizing；
(5) centrifugation：Potassium chloride after by condensing crystallizing carries out centrifugal dehydration treatment, centrifuge mother liquor and potassium chloride raw material
Mixing circulation is used；
(6) dry：Potassium chloride after by centrifugal dehydration is dried, and obtains high-purity food-grade potassium chloride.
In step (3), the flow that pumps into of Klorvess Liquid is 10-25m3/ h, the pH of Klorvess Liquid is 9-11, during absorption
Between be 0.5-2h.
In step (3), described ion exchange resin is that storng-acid cation exchange resin or Subacidity cation are exchanged
Resin, preferably storng-acid cation exchange resin.
In step (4), the temperature of described condensing crystallizing is 70-120 DEG C.
The present invention produces food-grade potassium chloride by ion exchange resin adsorption and purification, purified industrial potassium chloride.Ion is handed over
Change resin treatment ability big, can optionally remove sodium ion and heavy metal ion, renewable use, long working life, operation
Expense is relatively low.Ion exchange resin has higher mechanical strength simultaneously, and stable chemical nature, service life are longer.The present invention
Technological process simple, can obtain that particle is big and uniform high-grade potassium chloride.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
With reference to embodiment, the present invention is described further.
Embodiment 1
To render in dissolving tank under the potassium chloride room temperature of content (weight content) >=96%, dissolving under stirring is obtained
Klorvess Liquid, solution are stored in after being filtered through filter in dashpot, and Klorvess Liquid is pumped into Subacidity cation
Exchange resin column is adsorbed, and flow controls 10m3/ h, pH control in 11, time swap 0.5h, by absorption after potassium chloride molten
Liquid sends into crystallizer, is to carry out condensing crystallizing at 120 DEG C in temperature, and the potassium chloride slurry that crystallization is completed is drained into centrifuge to be carried out
Dehydrating operations, centrifuge mother liquor are transported to dissolving tank recycling.After Potassium Chloride Product after centrifugal dehydration is through fluidized bed drying, obtain
To the food-grade potassium chloride of purity >=99.1%, wherein sodium content is 0.3%, and, as 2ppm, arsenic is not for content of beary metal (being counted with Pb)
Detection.
Embodiment 2
To render in dissolving tank under the potassium chloride room temperature of content (weight content) >=96%, dissolving under stirring is obtained
Klorvess Liquid, solution are stored in after being filtered through filter in dashpot, and Klorvess Liquid is pumped into highly acidic cation
Exchange resin column carries out adsorption process, and flow controls 25m3/ h, pH control in 9, time swap 2.0h, by absorption after potassium chloride
Solution sends into crystallizer, is to carry out condensing crystallizing at 120 DEG C in temperature, and the potassium chloride slurry that crystallization is completed is drained into centrifuge and enters
Row dehydrating operations, centrifuge mother liquor are transported to dissolving tank recycling.After Potassium Chloride Product after centrifugal dehydration is through fluidized bed drying,
Obtain the food-grade potassium chloride of purity >=99.5%, wherein sodium content is 0.2%, content of beary metal (being counted with Pb) as 2ppm, arsenic
Do not detect.
Embodiment 3
To render in dissolving tank under the potassium chloride room temperature of content (weight content) >=96%, dissolving under stirring is obtained
Klorvess Liquid, solution are stored in after being filtered through filter in dashpot, with by Klorvess Liquid pump into highly acid sun from
Sub-exchange resin post carries out adsorption process, and flow controls 15m3/ h, pH control in 11, time swap 2.0h, by absorption after chlorine
Change potassium solution and send into crystallizer, be at 70 DEG C, to carry out condensing crystallizing in temperature, crystallize the potassium chloride slurry for completing and be drained into centrifugation
Machine carries out dehydrating operations, and centrifuge mother liquor is transported to dissolving tank recycling.Potassium Chloride Product after centrifugal dehydration is dry through fluid bed
After dry, the food-grade potassium chloride of purity >=99.3% is obtained, and wherein sodium content is 0.2%, and content of beary metal (in terms of Pb) is
2ppm, arsenic are not detected.
According to the regulation of GB25585-2010, food-grade potassium chloride needs the condition for meeting specific as follows：PH value is by examination
Test, iodine is with bromine by test, arsenic≤2ppm, heavy metal≤5ppm, loss on drying≤1.0%, sodium≤0.5%.Gained of the present invention
Food-grade potassium chloride fully meet above-mentioned requirements.
Claims (4)
1. a kind of production method of high-purity food-grade potassium chloride, it is characterised in that comprise the following steps that：
(1) dissolve：Under room temperature, by potassium chloride raw material stirring and dissolving；
(2) filter：Klorvess Liquid is filtered, sediment is removed；
(3) ion exchange resin adsorption and purification：Klorvess Liquid is pumped into ion exchange resin column to be adsorbed；
(4) condensing crystallizing：Klorvess Liquid after by absorption carries out condensing crystallizing；
(5) centrifugation：Potassium chloride after by condensing crystallizing carries out centrifugal dehydration treatment, and centrifuge mother liquor is mixed with potassium chloride raw material
Recycle；
(6) dry：Potassium chloride after by centrifugal dehydration is dried, and obtains high-purity food-grade potassium chloride.
2. the production method of high-purity food-grade potassium chloride according to claim 1, it is characterised in that in step (3), chlorination
The flow that pumps into of potassium solution is 10-25m3/ h, the pH of Klorvess Liquid is 9-11, and adsorption time is 0.5-2h.
3. the production method of high-purity food-grade potassium chloride according to claim 1, it is characterised in that in step (3), described
Ion exchange resin be storng-acid cation exchange resin or weak-acid cation-exchange resin.
4. the production method of high-purity food-grade potassium chloride according to claim 1, it is characterised in that in step (4), described
Condensing crystallizing temperature be 70-120 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064836.3A CN106495189A (en) | 2016-11-28 | 2016-11-28 | A kind of production method of high-purity food-grade potassium chloride |
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| CN201611064836.3A CN106495189A (en) | 2016-11-28 | 2016-11-28 | A kind of production method of high-purity food-grade potassium chloride |
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| CN106495189A true CN106495189A (en) | 2017-03-15 |
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| CN201611064836.3A Pending CN106495189A (en) | 2016-11-28 | 2016-11-28 | A kind of production method of high-purity food-grade potassium chloride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498431A (en) * | 2019-08-13 | 2019-11-26 | 广州怡和生物科技有限公司 | A kind of preparation method of high-purity spherical shape potassium chloride |
| WO2021009503A1 (en) * | 2019-07-15 | 2021-01-21 | Klinge Chemicals Limited | Process for purifying potassium chloride |
| CN113443639A (en) * | 2021-06-25 | 2021-09-28 | 江阴润玛电子材料股份有限公司 | Preparation process of electronic-grade potassium hydroxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850991A (en) * | 2010-01-14 | 2010-10-06 | 河北工业大学 | Method for preparing potassium chloride from seawater |
| CN105060315A (en) * | 2015-09-06 | 2015-11-18 | 华陆工程科技有限责任公司 | Method for producing food-grade potassium chloride by adopting adsorption process |
| CN205151795U (en) * | 2015-09-06 | 2016-04-13 | 华陆工程科技有限责任公司 | Adopt device that adsorbs technology production food level potassium chloride |
-
2016
- 2016-11-28 CN CN201611064836.3A patent/CN106495189A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850991A (en) * | 2010-01-14 | 2010-10-06 | 河北工业大学 | Method for preparing potassium chloride from seawater |
| CN105060315A (en) * | 2015-09-06 | 2015-11-18 | 华陆工程科技有限责任公司 | Method for producing food-grade potassium chloride by adopting adsorption process |
| CN205151795U (en) * | 2015-09-06 | 2016-04-13 | 华陆工程科技有限责任公司 | Adopt device that adsorbs technology production food level potassium chloride |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021009503A1 (en) * | 2019-07-15 | 2021-01-21 | Klinge Chemicals Limited | Process for purifying potassium chloride |
| CN110498431A (en) * | 2019-08-13 | 2019-11-26 | 广州怡和生物科技有限公司 | A kind of preparation method of high-purity spherical shape potassium chloride |
| CN113443639A (en) * | 2021-06-25 | 2021-09-28 | 江阴润玛电子材料股份有限公司 | Preparation process of electronic-grade potassium hydroxide |
| CN113443639B (en) * | 2021-06-25 | 2023-08-04 | 江阴润玛电子材料股份有限公司 | Preparation process of electronic grade potassium hydroxide |
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Application publication date: 20170315 |