CN107140658A - A kind of preparation method of high-purity potassium hydroxide product - Google Patents
A kind of preparation method of high-purity potassium hydroxide product Download PDFInfo
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- CN107140658A CN107140658A CN201710525047.3A CN201710525047A CN107140658A CN 107140658 A CN107140658 A CN 107140658A CN 201710525047 A CN201710525047 A CN 201710525047A CN 107140658 A CN107140658 A CN 107140658A
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- potassium hydroxide
- purity
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- potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
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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
Abstract
The present invention relates to a kind of preparation method of high-purity potassium hydroxide product, comprise the following steps：(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；(2) toward complexing agent is continuously added in filtrate, freeze and keep liquid condition, produce water and potassium hydroxide crystallization；(3) crystallization of hydronium(ion) potassium oxide is collected, takes its heating to dissolve the potassium hydroxide solution product for obtaining high-purity, and heating, drying then obtains high-purity solid potassium hydroxide product under inert gas shielding.Compared with prior art, the present invention has the advantages that purity height, corrosivity are small, simple to operate, dangerous small.
Description
Technical field
The present invention relates to a kind of preparation method of potassium hydroxide product, more particularly, to a kind of high-purity potassium hydroxide product
Preparation method.
Background technology
In the gold-tinted process stage of touch-screen industry, photoresist developing and stripping process are required for using high-purity potassium hydroxide
Solution.The height of potassium hydroxide purity has a great impact to the quality of back segment product.Technical grade potassium hydroxide has been met not
Require.Therefore, it is necessary to be purified to technical grade potassium hydroxide, quality is lifted.
Chinese patent ZL96110804.5 is related to the fluorine-containing cation exchange membrane of electrolysis and by using the cation exchange
The method that film hydrolyzes Klorvess Liquid as barrier film and produces potassium hydroxide of high purity, the method energy consumption is larger, and cost is high.
ZL200810147324.2 is related to a kind of method of purifying potassium hydroxide aqueous solution of the utilization low-carbon alcohols extraction rich in sila matter, most
Low-carbon alcohols are removed by being separated eventually and obtain the potassium hydroxide aqueous solution that sila matter is reduced.The method is not related to just for impurity silicon
And to the removal of other foreign ions.ZL201010576437.1 discloses one kind, and that potassium metaborate is dissolved into sodium hydroxide is water-soluble
In liquid, by being heated to reflux, separation of solid and liquid obtains solid potassium hydroxide, and the method technological process is complicated, and energy consumption is big, is not related in patent
And to potassium hydroxide purity problem.Chinese patent ZL201010586303.8, which is disclosed, utilizes the production of fluoric-containing acid low-temperature decomposing of potassium feldspar
Potassium hydroxide technique, potassium hydroxide product is made by cyclic absorption, separation of solid and liquid, evaporation and concentration, dehydration.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of high-purity potassium hydroxide
The preparation method of product.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward complexing agent is continuously added in filtrate, freeze and keep liquid condition, produce water and potassium hydroxide crystallization；
(3) crystallization of hydronium(ion) potassium oxide is collected, takes its heating to dissolve the potassium hydroxide solution product for obtaining high-purity, and
Heating, drying then obtains high-purity solid potassium hydroxide product under inert gas shielding.
As preferred embodiment, described water and potassium hydroxide crystallization are a hydronium(ion) potassium oxide, two hydrated hydroxides
Change potassium or/and four hydronium(ion) potassium oxides.According to the adjustment of proportioning and cryogenic temperature to ultra-pure water, can selectivity generation one
Hydronium(ion) potassium oxide, two hydronium(ion) potassium oxides and four hydronium(ion) potassium oxides.It is furthermore preferred that described water and potassium hydroxide crystallization are
One hydronium(ion) potassium oxide.
As preferred embodiment, described complexing agent is organophosphor acids complexing agent, and it primarily serves chelating absorption
Impurity metal ion, and it is at dissolved state, it is to avoid potassium hydroxide can take impurity metal ion out of when crystallizing, with more preferable
Improve potassium hydroxide product design.
As preferred embodiment, the addition of described complexing agent is 0.1~5wt%.
As preferred embodiment, the temperature of freezing is -50~-10 DEG C.
As preferred embodiment, the potassium hydroxide quality content in the potassium hydroxide solution product of the high-purity is
The mass content of potassium hydroxide in 20-50%, the high-purity solid potassium hydroxide product is more than 99%, all potassium hydroxide
In product, arsenic content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Compared with prior art, the present invention uses industrial potassium hydroxide for raw material, by filtering pre- removal of impurities, then adds network
Mixture removes heavy metal plasma impurity, finally by the mode of freezing and crystallizing, by potassium hydroxide in the way of crystalline hydrate with
Remaining impurity is separated, and obtained potassium hydroxide product purity is high, corrosivity is small, and whole technological operation is simple, dangerous
It is small etc..
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 2wt% is continuously added in filtrate, freezed at -30 DEG C and keep liquid condition, produce water and hydrogen
Potassium oxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, the potassium hydroxide solution product for obtaining high-purity is dissolved in heating.
After after testing, the potassium hydroxide quality content in the potassium hydroxide solution product of above-mentioned high-purity is 40% or so,
Arsenic content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 2
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 0.1wt% is continuously added in filtrate, freezed at -50 DEG C and keep liquid condition, produce water and
Potassium hydroxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, lower heating, drying is enclosed in nitrogen protective atmosphere, that is, obtains high-purity solid hydrogen-oxygen
Change potassium product.
After after testing, the mass content of the potassium hydroxide in above-mentioned high-purity solid potassium hydroxide product is more than 99%, arsenic
Content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 3
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 5wt% is continuously added in filtrate, freezed at -10 DEG C and keep liquid condition, produce water and hydrogen
Potassium oxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, the potassium hydroxide solution product for obtaining high-purity is dissolved in heating.
After after testing, the potassium hydroxide quality content in the potassium hydroxide solution product of above-mentioned high-purity is 50% or so,
Arsenic content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 4
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 1wt% is continuously added in filtrate, freezed at -40 DEG C and keep liquid condition, produce water and hydrogen
Potassium oxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, lower heating, drying is enclosed in nitrogen protective atmosphere, that is, obtains high-purity solid hydrogen-oxygen
Change potassium product.
After after testing, the mass content of the potassium hydroxide in above-mentioned high-purity solid potassium hydroxide product is more than 99%, arsenic
Content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 5
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 2wt% is continuously added in filtrate, freezed at -20 DEG C and keep liquid condition, produce water and hydrogen
Potassium oxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, the potassium hydroxide solution product for obtaining high-purity is dissolved in heating.
After after testing, the potassium hydroxide quality content in the potassium hydroxide solution product of above-mentioned high-purity is 20% or so,
Arsenic content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 6
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 4wt% is continuously added in filtrate, freezed at -15 DEG C and keep liquid condition, produce water and hydrogen
Potassium oxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, lower heating, drying is enclosed in nitrogen protective atmosphere, that is, obtains high-purity solid hydrogen-oxygen
Change potassium product.
After after testing, the mass content of the potassium hydroxide in above-mentioned high-purity solid potassium hydroxide product is more than 99%, arsenic
Content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 7
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 0.8wt% is continuously added in filtrate, freezed at -45 DEG C and keep liquid condition, produce water and
Potassium hydroxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, the potassium hydroxide solution product for obtaining high-purity is dissolved in heating.
After after testing, the potassium hydroxide quality content in the potassium hydroxide solution product of above-mentioned high-purity is 30% or so,
Arsenic content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
Embodiment 8
A kind of preparation method of high-purity potassium hydroxide product, comprises the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward the complexing agent that 1.5wt% is continuously added in filtrate, freezed at -25 DEG C and keep liquid condition, produce water and
Potassium hydroxide is crystallized；
(3) crystallization of hydronium(ion) potassium oxide is collected, lower heating, drying is enclosed in nitrogen protective atmosphere, that is, obtains high-purity solid hydrogen-oxygen
Change potassium product.
After after testing, the mass content of the potassium hydroxide in above-mentioned high-purity solid potassium hydroxide product is more than 99%, arsenic
Content is less than 0.00001wt%, and all content of beary metal are less than 0.00001wt%.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel are according to the announcement of the present invention, and not departing from improvement and modification that scope made all should be the present invention's
Within protection domain.
Claims (7)
1. a kind of preparation method of high-purity potassium hydroxide product, it is characterised in that comprise the following steps：
(1) industrial potassium hydroxide is taken to be dissolved in ultra-pure water, agitation and filtration removal of impurities；
(2) toward complexing agent is continuously added in filtrate, freeze and keep liquid condition, produce water and potassium hydroxide crystallization；
(3) crystallization of hydronium(ion) potassium oxide is collected, takes its heating to dissolve the potassium hydroxide solution product for obtaining high-purity, and lazy
Heating, drying then obtains high-purity solid potassium hydroxide product under property gas shield.
2. a kind of preparation method of high-purity potassium hydroxide product according to claim 1, it is characterised in that described water and
Potassium hydroxide crystallization is a hydronium(ion) potassium oxide, two hydronium(ion) potassium oxides or/and four hydronium(ion) potassium oxides.
3. a kind of preparation method of high-purity potassium hydroxide product according to claim 2, it is characterised in that described water and
Potassium hydroxide crystallization is a hydronium(ion) potassium oxide.
4. a kind of preparation method of high-purity potassium hydroxide product according to claim 1, it is characterised in that described complexing
Agent is organophosphor acids complexing agent.
5. a kind of preparation method of high-purity potassium hydroxide product according to claim 1, it is characterised in that described complexing
The addition of agent is 0.1~5wt%.
6. a kind of preparation method of high-purity potassium hydroxide product according to claim 1, it is characterised in that the temperature of freezing
For -50~-10 DEG C.
7. a kind of preparation method of high-purity potassium hydroxide product according to claim 1, it is characterised in that the high-purity
Potassium hydroxide solution product in potassium hydroxide quality content be 20-50%, in the high-purity solid potassium hydroxide product
The mass content of potassium hydroxide be more than 99%, in all potassium hydroxide products, arsenic content is less than 0.00001wt%, Suo Youchong
Tenor is less than 0.00001wt%.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100989A (en) * | 1986-02-28 | 1987-09-30 | 罗纳·布朗克化学股份有限公司 | The method of purification of barium salt |
| CN1978321A (en) * | 2005-11-29 | 2007-06-13 | 高崧耀 | Process for producing high-purity potassium chloride |
| CN101659428A (en) * | 2008-08-26 | 2010-03-03 | 天津市黎虹化工有限公司 | Process for producing high-purity potassium chloride |
| CN102583453A (en) * | 2011-08-31 | 2012-07-18 | 四川长和华锂科技有限公司 | Industrial method for producing battery-grade lithium carbonate or high-purity lithium carbonate |
| CN102826576A (en) * | 2011-09-19 | 2012-12-19 | 四川长和华锂科技有限公司 | Method for industrially producing industrial, cell-grade or high-purity lithium hydroxide monohydrate |
| CN104016376A (en) * | 2014-06-25 | 2014-09-03 | 苏州晶瑞化学有限公司 | Continuous production method of high-purity potassium hydroxide water solution |
-
2017
- 2017-06-30 CN CN201710525047.3A patent/CN107140658A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100989A (en) * | 1986-02-28 | 1987-09-30 | 罗纳·布朗克化学股份有限公司 | The method of purification of barium salt |
| CN1978321A (en) * | 2005-11-29 | 2007-06-13 | 高崧耀 | Process for producing high-purity potassium chloride |
| CN101659428A (en) * | 2008-08-26 | 2010-03-03 | 天津市黎虹化工有限公司 | Process for producing high-purity potassium chloride |
| CN102583453A (en) * | 2011-08-31 | 2012-07-18 | 四川长和华锂科技有限公司 | Industrial method for producing battery-grade lithium carbonate or high-purity lithium carbonate |
| CN102826576A (en) * | 2011-09-19 | 2012-12-19 | 四川长和华锂科技有限公司 | Method for industrially producing industrial, cell-grade or high-purity lithium hydroxide monohydrate |
| CN104016376A (en) * | 2014-06-25 | 2014-09-03 | 苏州晶瑞化学有限公司 | Continuous production method of high-purity potassium hydroxide water solution |
Non-Patent Citations (3)
| Title |
|---|
| 潘欣艾: "光电/核电级高纯硼酸的制备及结晶形貌研究", <中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑> * |
| 韩长阳等: "《精细无机化学品制造技术》", 31 August 2008 * |
| 马祥伟等: "氢氧化镁络合除钡工艺初探", 《盐业与化工》 * |
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