CN1335266A - Production process of high-activity spherical nickel hydroxide - Google Patents
Production process of high-activity spherical nickel hydroxide Download PDFInfo
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- CN1335266A CN1335266A CN 00110683 CN00110683A CN1335266A CN 1335266 A CN1335266 A CN 1335266A CN 00110683 CN00110683 CN 00110683 CN 00110683 A CN00110683 A CN 00110683A CN 1335266 A CN1335266 A CN 1335266A
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Abstract
The present invention relates to the production of high activity spherical nickel hydroxide for nickel battery. The present invention features that the stirring speed in the reactor is regulated to 160-500 rpm so that the nickel hydroxide is controlled to grow into spherical or quasi-spherical crystal with peak width at half-height of XRD (101) plane over 0.85 deg, bulk density of 1.5-1.8 g/ml, and tap density of 2.1-2.4 g/ml. The present invention has the features of high yield, high density and long life of the product.
Description
The present invention relates to the production method of the activity spherical nickle hydroxide that metal hydride-nickel battery uses.Mainly be exactly nickel hydroxide powder by adjust the reaction system stirring velocity reach the control nickel hydroxide grow up to sphere or class sphere, XRD curve (101) face halfwidth more than 0.85 degree, loose density is the method for 1.5-1.8g/ml.
Nickel hydroxide powder mainly is used as the positive electrode active materials of NI-G and nickel metal hydride battery and alkaline cell etc., general method for making is at present: the nickel salt aqueous solution that the caustic solution of caustic soda and Ke Xingjia etc. is acted on nickelous nitrate and single nickel salt etc. under the prerequisite that has ammoniacal liquor to exist, in reaction process, concentration by adding various materials in the fixed system and add-on, system pH value, stirring velocity, produce sphere or class ball-shape nickel hydroxide precipitation, obtain nickel hydroxide through operations such as solid-liquid separation, washing, dryings then.The nickel hydroxide that obtains like this is difficult to satisfy the requirement of high tamped density of modern MH-Ni battery and high-capacitance.
Day disclosure special permission spy opens the manufacture method that flat 8-119636 has announced nickel hydroxide: with nickel salt solution, caustic solution, the continuous injecting reactor of ammonia soln and stirring simultaneously.The pH value of control reaction system in the reaction process.When question response liquid reaches the reaction vessel capacity, remove medium liquid in the reaction system, make reaction solution minimizing in the reaction system, continue to inject nickel salt solution, caustic solution, ammonia soln then.After repeatable operation, generate nickel hydroxide.Obtain the product tap density and reach 1.9-2.2g/ml.Though the production control method of this nickel hydroxide can access the product that has than high tap density, but still can not satisfy of the requirement of modern MH-Ni battery with activity spherical nickle hydroxide XRD curve (101) face halfwidth, and troublesome poeration, production efficiency is low.
Day disclosure special permission spy opens the up-to-date method for making that flat 9-283135 has announced nickel hydroxide: at the synthetic groove that is having synthetic nickel ammine, the reactor that the nickel hydroxide reaction solution overflows continuously, its reaction obtains the nickel hydroxide tap density and reaches 2.0g/ml, and its interior tissue is periodical change.The product that this production control method obtains still can not satisfy the modern MH-Ni battery needs with high electrical performance, and its quality product is unsettled in one-period, and control is unstable.
Purpose of the present invention just provides and a kind ofly can satisfy that XRD curve (101) the face halfwidth that metal hydride-nickel battery uses is big, the production method of activity spherical nickle hydroxide constant product quality, simple to operate.
The object of the present invention is achieved like this: comprise nickel salt solution and alkaline solution and concentrated ammonia solution are imported reactor continuously, by fixation reaction substrate concentration, feed rate, pH value, the reinforced mol ratio of ammonia nickel, temperature of reaction in the reaction system, and the production method of overflowing from overflow port continuously, the stirring velocity that it is characterized in that adjusting material in reactor is 160-500rpm, reach the control nickel hydroxide grow up to sphere or class sphere, XRD curve (101) face halfwidth more than 0.85 degree, loose density is that 1.5-1.8g/ml, tap density are 2.1-2.4g/ml.
Major advantage of the present invention:
1, reaction conditions of the present invention is easy to control, and manual operations can be produced MH-Ni battery the high reactivity nickel hydroxide sphere or the class spherical powder product of stable performance.Reactor throughput height, one 1 cubic metre reactor daily output sphere or class ball-shape nickel hydroxide are that powder can reach 250kg, its optimum yield is 150-180kg.Because product is sphere or class sphere, it is very convenient to wash.
2, the nickel hydroxide that the present invention produced is that powder is sphere or class sphere, and loose density and tap density height can reach 1.5-1.8g/ml, 2.1-2.4g/ml respectively.This powder before making electrode during the furnishing pasty state, good fluidity, tamped density height.
3, the nickel hydroxide product halfwidth produced of working condition of the present invention is big, and more than 0.85 degree, its best halfwidth scope is between the 0.85-1.1 degree.This product is made loading capacity height behind the MH-Ni battery, and mean lifetime reached more than 500 weeks.
Fig. 1 is the form of the embodiment of the invention 1.
Below technical scheme of the present invention is described further:
Reactant is nickel salt solution (the i.e. single nickel salt salts solution of 1.7-2.1mol/l (mol), also one or more mixing salt solutions of single nickel salt and rose vitriol, zinc sulfate, the nickel salt solution volumetric molar concentration is meant the volumetric molar concentration sum of nickel salt, zinc salt, cobalt salt) and density be the strong aqua of 0.88-0.92g/ml and the caustic solution of 8-9mol/l.Reactant nickel salt solution and alkaline solution and concentrated ammonia solution are by 1.0: 1.7-2.1: the 09-1.2 mol ratio is determined the relative discharge between them.Temperature of reaction is a certain fixed value between 50-65 degree centigrade and be controlled at ± 2 degrees centigrade.The pH value of reaction solution is selected a certain fixed value between 11.0-12.0, and the pH value amplitude that reaches control solution by adjustment alkaline solution feed rate is ± 0.2.The stirring velocity of adjusting material in reactor is 160-500rpm, reach the control nickel hydroxide grow up to sphere or class sphere, more than XRD curve (101) face halfwidth 0.85 degree, loose density is 1.5-1.8g/ml, tap density is 2.1-2.4g/ml.
Nickel hydroxide powder can be one or more a coprecipitation powder of simple nickel hydroxide powder or the cobaltous hydroxide that contains coprecipitation in nickel hydroxide powder, zinc hydroxide.
Embodiment of the present invention 1:
1 cubic metre of reactor volume, reaction soln are the mixing salt volumetric molar concentration 2.0mol/l of single nickel salt, rose vitriol, zinc sulfate, and the sodium hydroxide solution volumetric molar concentration is 9.0mol/l, and ammoniacal liquor density is 0.88-0.92g/ml.The pH value of reaction system is controlled at 11.6 ± 0.2, and temperature of reaction is 58 ± 1 degrees centigrade.The rate of addition mol ratio of nickel salt and caustic solution and ammoniacal liquor is 1: 2.15: 1.1 in the reaction process, and adjusting the stirring velocity scope in the reaction is 280-350rpm.Reaction back nickel hydroxide particle is spherical.Monitoring continuously 20 day data (data of test in two days) are seen Fig. 1.
Embodiment of the present invention 2:
1 cubic metre of reactor volume, reaction soln are the mixing salt volumetric molar concentration 2.1mol/l of single nickel salt, rose vitriol, zinc sulfate, and the sodium hydroxide solution volumetric molar concentration is 8.4mol/l, and ammoniacal liquor density is 0.892g/ml.Sodium hydroxide, nickel salt, the reinforced mol ratio of ammonia soln are 2.1: 1.0: 1.1 in the reaction.The pH value of reaction system is controlled at 11.5 ± 0.1, and temperature of reaction is 60 ± 2 degrees centigrade.The powerful stirring in the reaction, stirring velocity is 480rpm, the reaction solution mean residence time is 20 hours.Reaction back nickel hydroxide is that particle is spherical and class sphere, and loose density is 1.72g/ml, and tap density is 2.32g/ml, and median size 10.4 μ m, particle diameter scope 1-50 μ m, (101) face halfwidth are 0.95 degree, and making and testing the life-span behind the battery was 580 weeks.
Claims (3)
1, the production method of activity spherical nickle hydroxide comprises nickel salt solution and alkaline solution and concentrated ammonia solution is imported reactor continuously, by pH value in fixation reaction substrate concentration, feed rate, the reaction system, the reinforced mol ratio of ammonia nickel, temperature of reaction, and the production method of overflowing from overflow port continuously, it is characterized in that adjusting the material in reactor stirring velocity is 160-500rpm, reach the control nickel hydroxide grow up to sphere or class sphere, XRD curve (101) face halfwidth more than 0.85 degree, loose density is that 1.5-1.8g/ml, tap density are 2.1-2.4g/ml.
2, the production method of activity spherical nickle hydroxide according to claim 1, it is characterized in that adjusting the material in reactor stirring velocity is 280-350rpm.
3, the production method of activity spherical nickle hydroxide according to claim 1, it is characterized in that adjusting the material in reactor stirring velocity is 480rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110683 CN1335266A (en) | 2000-07-20 | 2000-07-20 | Production process of high-activity spherical nickel hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00110683 CN1335266A (en) | 2000-07-20 | 2000-07-20 | Production process of high-activity spherical nickel hydroxide |
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| CN1335266A true CN1335266A (en) | 2002-02-13 |
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| CN 00110683 Pending CN1335266A (en) | 2000-07-20 | 2000-07-20 | Production process of high-activity spherical nickel hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328173C (en) * | 2002-05-09 | 2007-07-25 | 辽宁浩普科技发展有限公司 | Nanometer geode-type nickelous hydroxide producing method and apparatus thereof for MH-Ni cells as power |
-
2000
- 2000-07-20 CN CN 00110683 patent/CN1335266A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328173C (en) * | 2002-05-09 | 2007-07-25 | 辽宁浩普科技发展有限公司 | Nanometer geode-type nickelous hydroxide producing method and apparatus thereof for MH-Ni cells as power |
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