CN101481123A - Preparation of potassium hydrate - Google Patents

Preparation of potassium hydrate Download PDF

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Publication number
CN101481123A
CN101481123A CNA2009101110262A CN200910111026A CN101481123A CN 101481123 A CN101481123 A CN 101481123A CN A2009101110262 A CNA2009101110262 A CN A2009101110262A CN 200910111026 A CN200910111026 A CN 200910111026A CN 101481123 A CN101481123 A CN 101481123A
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CN
China
Prior art keywords
potassium hydroxide
filtrate
ammonia
preparation
reaction
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Pending
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CNA2009101110262A
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Chinese (zh)
Inventor
钟劲光
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XIAMEN YIGONG CHEMICAL TECHNOLOGY Co Ltd
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XIAMEN YIGONG CHEMICAL TECHNOLOGY Co Ltd
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Priority to CNA2009101110262A priority Critical patent/CN101481123A/en
Publication of CN101481123A publication Critical patent/CN101481123A/en
Pending legal-status Critical Current

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  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The invention provides a method for preparing potassium hydroxide, which relates to alkali metal hydroxide. The invention provides a potassium hydroxide preparing method with low energy consumption and small investment and using the electroless method. The method comprises the following steps: dissolving a KCl solution in water to form a saturated solution, adding Ni(OH)2; introducing ammonia gas or adding liquid ammonia to the saturated solution for reaction so that the free ammonia concentration in the solution is between 20 percent and 50 percent to obtain a crystal mush; centrifugally filtering or filter pressing the crystal mush formed by reaction to obtain the filtrate which is a potassium hydroxide aqua ammonia; heating the filtrate to evaporate so that the ammonia inside the filtrate is evaporated completely to obtain the filtrate after the ammonia evaporation; filtering the filtrate after the ammonia evaporation to obtain the liquid potassium hydroxide product, and producing the solid product of potassium hydroxide by further heating and dehydrating.

Description

A kind of preparation method of potassium hydroxide
Technical field
The present invention relates to a kind of alkali metal hydroxide, especially relate to a kind of preparation method of potassium hydroxide.
Background technology
Potassium hydroxide is a kind of important chemical material, and existing industry all adopts the method for electrolytic chlorination potassium to produce potassium hydroxide.Though the potassium hydroxide that electrolysis process is produced pollutes less, the quality height, owing to demanding strict technology of electrolyzer, the processing and the application apparatus of simultaneously necessary supporting chlorine, so one-time investment is big, and to consume a large amount of electric energy.
Publication number is that the application for a patent for invention of CN1410597 discloses a kind of method for preparing potassium hydroxide, this method belongs to the liquid metal katholysis, used in the electrolyzer by metal such as gallium, indium, tin, bismuth, silver or the low melting point alloy that becomes of certain several metal group wherein, an insulating barrier is vertically inserted on top at electrolyzer, to liquid alloy, separated by spaces is become tank room and finished room, and liquid alloy can be in the insulcrete current downflow, anode is arranged at tank room top, the negative electrode that the bottom has liquid alloy to constitute.Electrolytic anode makes the chlorion in the Klorvess Liquid become chlorine and emits, the negative electrode of electrolyzer is the liquid alloy layer, it attracts potassium ion and makes it reduction formation potassium-sodium alloy neat, and potassium-sodium alloy moves to another zone together and generates potassium hydroxide with the water effect, and releasing hydrogen gas.
Notification number is that the patent of invention of CN1147567 discloses a kind of electrolytic cationic exchange membrane that is used for, it comprises the two-layer at least fluoro-containing copolymer film that has sulfonic acid group, it is characterized in that the first layer faces anode, it is to be made by following monomer (A), (B) and the three-component polymer that (C) generates, its thickness is 50 to 150 μ m, and second layer thickness is 50 to 300 μ m:(A) CF 2=CF (OCF 2CFCF 3) mO (CF 2) nSO 3M$ is m=0 or 1 wherein, and n=1 to 5, M are hydrogen or basic metal, $ (B) CF 2=CF 2, (C) CF 2=CFO (CF 2CFO) mRf$$ is m=0 or 1 wherein, and Rf is C 1-10Perfluoroalkyl.
Summary of the invention
The objective of the invention is to produce the existing electrolyzer of potassium hydroxide at existing electrolysis process demands strict technology, the processing and the application apparatus of necessary supporting chlorine, one-time investment is big, and consume deficiencies such as a large amount of electric energy, provide a kind of energy consumption low, less investment, adopt the preparation method of the potassium hydroxide of non-electrolysis process.
Primitive reaction principle of the present invention is: 2KCl+Ni (OH) 2+ 6NH 3=2KOH+Ni (NH 3) 6Cl 2↓.
The present invention includes following steps:
1), adds Ni (OH) with KCl formation saturated solution soluble in water 2, feed ammonia then or add liquefied ammonia and react, make the concentration of free ammonia in the solution reach 20%~50%, get magma;
2) magma centrifuging or the press filtration that the step 1) reaction is formed gets filtrate, and filtrate is potassium hydroxide aqua ammonia;
3) with the filtrate heating evaporation, the ammonia in the filtrate is evaporated fully, the filtrate after the ammonia still process;
4) filtrate after the ammonia still process is filtered, obtain the liquid potassium hydroxide product, further thermal dehydration can obtain the solid potassium hydroxide product.
The temperature of described reaction is preferably 0~50 ℃, and the pressure of reaction is preferably 0.1~1.5MPa, in molar ratio, and KCl: Ni (OH) 2Be preferably 2: 1.
Magma centrifuging or press filtration are preferably in centrifuging or press filtration under the air-tight state.
The filtrate heating evaporation is preferably risen to 120 ℃ with the temperature of filtrate.
After the magma centrifuging or press filtration with step 1) reaction formation, can get Ni (NH 3) 6Cl 2Filter cake adds the milk of lime heat treated again, recyclable NH 3And Ni (OH) 2Or use steam heating deamination, recyclable Ni (OH) 2And NH 4Cl.
Produce potassium hydroxide relatively with existing employing electrolysis process, because the present invention adopts KCl solution, Ni (OH) 2React with ammonia or liquefied ammonia, make the concentration of free ammonia in the solution reach 20%~50%, with magma centrifuging or the press filtration that obtains, again with filtrate (potassium hydroxide aqua ammonia) heating evaporation, filter, obtain required product, therefore fundamentally having overcome the existing electrolyzer of existing electrolysis process production potassium hydroxide demands strict technology, the processing and the application apparatus of necessary supporting chlorine, one-time investment is big, and consume deficiencies such as a large amount of electric energy, provide a kind of energy consumption low, less investment, adopt the method for the production potassium hydroxide of non-electrolysis process.
Embodiment
Embodiment 1
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, adding liquefied ammonia then while stirring, controlled temperature keep-ups pressure at 0.1MPa at 0 ℃, makes the concentration of free ammonia in the solution reach 20%.Magma centrifuging under air-tight state with reaction formation.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 93g, and thermal dehydration can be undertaken by traditional solid potassium hydroxide production technique.
Embodiment 2
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, feeding ammonia then while stirring, controlled temperature keep-ups pressure at 0.2MPa at 10 ℃, makes the concentration of free ammonia in the solution reach 50%.With the magma that reaction forms, centrifuging under air-tight state.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 99g.
Embodiment 3
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, feeding ammonia then while stirring, controlled temperature keep-ups pressure at 0.3MPa at 20 ℃, makes the concentration of free ammonia in the solution reach 30%.With the magma that reaction forms, centrifuging under air-tight state.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 95g.
Embodiment 4
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, feeding ammonia then while stirring, controlled temperature keep-ups pressure at 0.5MPa at 30 ℃, makes the concentration of free ammonia in the solution reach 35%.With the magma that reaction forms, centrifuging under air-tight state.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 87g.
Embodiment 5
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, feeding ammonia then while stirring, controlled temperature keep-ups pressure at 0.7MPa at 40 ℃, makes the concentration of free ammonia in the solution reach 30%.With the magma that reaction forms, centrifuging under air-tight state.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 85g.
Embodiment 6
With 149g KCl formation saturated solution soluble in water, add 93g Ni (OH) 2, feeding ammonia then while stirring, controlled temperature keep-ups pressure at 1.5MPa at 50 ℃, makes the concentration of free ammonia in the solution reach 30%.With the magma that reaction forms, centrifuging under air-tight state.Filter cake is recycled, the filtrate heating evaporation, and temperature is raised to 120 ℃, and the ammonia in the filtrate is evaporated fully.Filtrate after the ammonia still process obtains the liquid potassium hydroxide product after filtration, and further thermal dehydration can obtain solid potassium hydroxide product 81g.

Claims (6)

1. the preparation method of a potassium hydroxide is characterized in that may further comprise the steps:
1), adds Ni (OH) with KCl formation saturated solution soluble in water 2, feed ammonia then or add liquefied ammonia and react, make the concentration of free ammonia in the solution reach 20%~50%, get magma;
2) magma centrifuging or the press filtration that the step 1) reaction is formed gets filtrate, and filtrate is potassium hydroxide aqua ammonia;
3) with the filtrate heating evaporation, the ammonia in the filtrate is evaporated fully, the filtrate after the ammonia still process;
4) filtrate after the ammonia still process is filtered, obtain the liquid potassium hydroxide product, further thermal dehydration obtains the solid potassium hydroxide product.
2. the preparation method of a kind of potassium hydroxide as claimed in claim 1, the temperature that it is characterized in that described reaction is 0~50 ℃, the pressure of reaction is 0.1~1.5MPa.
3. the preparation method of a kind of potassium hydroxide as claimed in claim 1 is characterized in that in molar ratio KCl: Ni (OH) 2It is 2: 1.
4. the preparation method of a kind of potassium hydroxide as claimed in claim 1 is characterized in that magma centrifuging or press filtration centrifuging or press filtration under air-tight state.
5. the preparation method of a kind of potassium hydroxide as claimed in claim 1 is characterized in that with the filtrate heating evaporation it being that temperature with filtrate rises to 120 ℃.
6. the preparation method of a kind of potassium hydroxide as claimed in claim 1 is characterized in that described magma centrifuging or the press filtration that the step 1) reaction is formed, and gets Ni (NH 3) 6Cl 2Filter cake adds the milk of lime heat treated, reclaims NH 3And Ni (OH) 2Or use the steam heating deamination, reclaim Ni (OH) 2And NH 4Cl.
CNA2009101110262A 2009-02-11 2009-02-11 Preparation of potassium hydrate Pending CN101481123A (en)

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Application Number Priority Date Filing Date Title
CNA2009101110262A CN101481123A (en) 2009-02-11 2009-02-11 Preparation of potassium hydrate

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CN101481123A true CN101481123A (en) 2009-07-15

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102001684A (en) * 2010-11-25 2011-04-06 山东国邦药业股份有限公司 Method for preparing potassium hydroxide by using potassiummetaborate
CN112028129A (en) * 2020-08-18 2020-12-04 杭州逐真科技有限公司 Recycling treatment device and process for ferric trichloride etching solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102001684A (en) * 2010-11-25 2011-04-06 山东国邦药业股份有限公司 Method for preparing potassium hydroxide by using potassiummetaborate
CN112028129A (en) * 2020-08-18 2020-12-04 杭州逐真科技有限公司 Recycling treatment device and process for ferric trichloride etching solution

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Open date: 20090715