CN1078566C - Method and apparatus for making spherical nickel hydroxide with surface defect - Google Patents
Method and apparatus for making spherical nickel hydroxide with surface defect Download PDFInfo
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- CN1078566C CN1078566C CN98101504A CN98101504A CN1078566C CN 1078566 C CN1078566 C CN 1078566C CN 98101504 A CN98101504 A CN 98101504A CN 98101504 A CN98101504 A CN 98101504A CN 1078566 C CN1078566 C CN 1078566C
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Abstract
The present invention relates to a method for preparing nickel hydroxide having a surface defect spherical shape and a device thereof. Nickel salt containing doping substances and lye are continuously added into a reaction kettle positively mixed in a spraying mode under the certain pressure, the nickel hydroxide is generated by hydrolysis under the condition of a stable multi-section pH value, and a product is separated, washed and dried by two seconds. A stirrer is arranged in the used device, a spiral type stirring mode and an anchor type stirring mode can be used, and a material feeding port can adopt a spray head type structure or a coiled pipe type structure. An active product with high density and high electrization is obtained, and the product is an ideal anode active material of non-burning type nickel-cadmium cells and nickel-hydrogen cells.
Description
The present invention relates to a kind of manufacturing method and apparatus of nickel hydroxide.Specifically a kind of manufacturing has the method and apparatus with high reactivity, high-density hydrogen nickel oxide of defect structure.
Nickel hydroxide is used as the positive active material of non-sintered type nickel metal hydride battery, and it directly determines the amount of capacity and the use properties of ni-mh, nickel-cadmium cell.Since the eighties, countries in the world around the density that how to improve nickel hydroxide, improve its activity and carried out big quantity research.Studying carefully its manufacture method has two classes, and a class is the simple hydrolysis precipitator method, and this method is in the aqueous solution, allows nickel ion and alkalimetal oxide effect, and hydrolysis generates nickel hydroxide.The European patent of Japanese Matsushita Electric Industrial Industrial Co., Ltd application: EP0523284A2 (1993), proposed to make the method for high reactivity high-density ball-shape nickel hydroxide, to contain the single nickel salt and the aqueous sodium hydroxide solution reaction of cobalt, zinc, prepare by the nickel hydroxide spherical, that class is spherical and the part aspherical particle is formed by the control feed rate, median size is 10～15 microns.During this nickel hydroxide jolt ramming, its density can reach more than 2.0 grams per milliliters, reach as high as 2.3 grams per milliliters, and make the aperture account for 20～70% of all micropores greater than 30 micropore, but shortcoming be industrial how accurately spherical, non-sphere of control and class spheric generate ratio, and how the internal void of crystallization control particle is very difficult.
Another kind of is that nickel ammino Heshui is separated the precipitator method: Chinese patent is open: CN1107442A, announced that nickel ammino Heshui separates precipitation and produce the method for nickel hydroxide, these patent characteristics are in advance nickel salt solution to be added in the ammonia soln, join in the reactor simultaneously continuously, temperature, the pH value of control reaction system, the formation particle is 2～50 microns a ball-shape nickel hydroxide, its disadvantage is that the add-on of ammonia is too big, cause the production environment severe exacerbation, be difficult to reach environmental requirement.The open CN1075697A of Chinese patent also announced and utilized nickel ammino Heshui to separate the method that precipitation is produced ball-shape nickel hydroxide, and it is that the molar weight of ammonia in the control reaction system is 0.3～0.4 of a nickel molar weight.This method can obtain the ball-shape nickel hydroxide product, and loose density is 1.4～1.8 grams per milliliters, tap density 1.8～2.2 grams per milliliters.Though this method has reduced ammonia volume, even under reactor, the airtight situation of duct height, also difficulty avoids ammonia to overflow, and does not reach environmental requirement.Though this product tamped density is big, electro-chemical activity is lower, generally at 200 Milliampere Hours/below the gram, can't satisfy the requirement of contemporary ni-mh, nickel-cadmium cell industry.In addition, Japan's special permission is open, Te Kaiping 66-340427, reported in the presence of stable ammonia, ammonium, by controlling free nickel ion concentration 10～100 mg/litre, the adding speed of regulating nickel liquid, alkali lye still still can't resolve environmental issue, and control reaction process condition by the control nickel ion, realize difficulty.
The objective of the invention is to avoid existing shortcoming, propose a kind of production high-density simultaneously and highly active, the manufacture method and the device thereof of the ball-shape nickel hydroxide with defect structure of non-environmental-pollution.
The present invention can realize with the following method that making the ball-shape nickel hydroxide with surface imperfection is to be generated by adulterated nickel salt and alkali reaction, and product gets product through separation, washing and drying treatment.Dopant is one or more water-soluble cpdss of zinc, cobalt, cadmium, magnesium, manganese, yttrium, platinum, palladium, rhodium, indium, gallium, gold, lanthanum, neodymium, samarium, europium, ytterbium, silver element, nickel salt is single nickel salt or nickelous nitrate or nickelous chloride, add water jointly and be mixed with nickel salt solution, its concentration of dopant is 0.01～10.00% of a nickel salt solution, nickel salt concentration is 20～200 grams per liters, nickel salt solution hydrojet speed be 10～400 liters/time.Alkali is selected sodium hydroxide or potassium hydroxide for use, concentration of lye is 1～15 mol, hydrojet speed be 5.0～200 liters/time, temperature of reaction is 10～70 ℃, and controlling pH value with the add-on of alkali is 8.0～14.0, and reaction is under agitation carried out, stirring velocity is 20～150 rev/mins, resultant of reaction is dry under vacuum, and drying temperature is 50～120 ℃, and the time is 2～4 hours.
Produce the device of ball-shape nickel hydroxide with surface imperfection, constitute by intake chute, reactor, whizzer and loft drier, raw material nickel salt and alkali lye are respectively charged into intake chute, send into after the pressurization in the reactor with chuck heating and react, reaction product is separated and washing through whizzer, product adds the loft drier drying afterwards, obtains the product ball-shape nickel hydroxide at last.The reactor charging opening is a nozzle structure, and the reactor center is equipped with agitator, and the discharge port of reaction product is driveed above the shower nozzle of feed(raw material)inlet.
The present invention can also realize with following method: the add-on of used hotchpotch is: cobalt salt: 1.8～2 grams per liters, and/or yttrium salt: 0.5～0.6 grams per liter, and/or indium salt: 0.2～0.3 grams per liter, and/or zinc salt: 3～5 grams per liters, and/or cadmium salt: 3～5 grams per liters.
The raw materials spray pressure is 1～20 kg/cm
2Reaction should be controlled a stable pH value, is 8～10 in preceding 15 hours control pH value scopes of reacting, and back 15 hours, the control pH value was chosen as 11～14, and these 30 hours was first reaction time.Afterwards, every 40～60 hours, the pH value control numerical value that repeated for first reaction time.Reactant retention time in reactor is 5～100 hours, and Best Times is 50～76 hours.
Drying is carried out gradient control, 50～60 ℃ of dryings 1～2 hour, and 120 ℃ of dryings 1～3 hour.
In the reaction equipment therefor, nickel salt and alkali lye charging opening place respectively in the reactor, the reinforced shower nozzle of alkali lye in reactor above, the reinforced shower nozzle of nickel salt solution is below reactor.Spray structure adopts circular cone spray nozzle type and/or perforated tube, and/or the alveolar disk tubular construction.Agitator is made of two portions up and down, and top is the propeller formula, and the bottom is the anchor formula.
The present invention compares with existing method, has following advantage: produce the easy control of reaction conditions of nickel hydroxide, and simple to operate, can manual operations also can adopt automated job.The employing serialization is reinforced, has fundamentally upgraded traditional feed way, the production efficiency height, and 2 cubic metres of reactors daily output nickel hydroxide is more than 500 kilograms.Because control pH value condition does not produce colloidal precipitation, only needs once washing, primary drying has been simplified technical process.Material temperature-gradient method vacuum-drying under flow state has kept the good flowability of material, need not fragmentation and screening, has both simplified technology and has also saved facility investment.Aspect environmental protection, product sulfur-bearing acid group of the present invention is extremely low, can reduce to below 0.1%, has overcome present home products sulfur-bearing acid group greater than 0.3% shortcoming, and the present invention has avoided use ammonia or ammonium raw material again, and production environment is improved at all.Present method adopts the atomized water forming solution, the ball-shape nickel hydroxide rational size distribution that generates, the surface has defective, solved a manufacturing technology difficult problem that has high reactivity and high-density ball-shape nickel hydroxide simultaneously, product loose density 1.6～1.8 grams per milliliters, tap density 1.8～2.2 grams per milliliters, electro-chemical activity are 270～300 MAH/grams, the product of this present just international and domestic heavy body ni-mh and the active demand of nickel-cadmium cell institute.
The drawing of accompanying drawing of the present invention is described as follows:
Fig. 1 is a reaction unit schematic flow sheet of the present invention;
Fig. 2 is the nickel hydroxide electron-microscope scanning figure that present city field boundary is sold;
Fig. 3 amplifies 1000 times electron-microscope scanning figure for product nickel hydroxide of the present invention;
Fig. 4 is 1000 times of electron-microscope scanning figure of the another kind of nickel hydroxide product of the present invention;
Fig. 5 is the electron-microscope scanning figure of 1000 times of the another kind of product nickel hydroxides of the present invention.
Below in conjunction with accompanying drawing the embodiment of the invention is described, the manufacturing process of its nickel hydroxide and equipment major technique are that nickel salt and the alkaline solution that will have hotchpotch spray in the reactor of forcing to stir 3 through ejiction opening, at stable pH value, under the certain temperature, the atomizing hydrolysis forms spherical nickel hydroxide particle, by regulating alkali lye atomizing hydrolysis rate, make nickel hydroxide generate 6～12 microns particle, scope is wide and distribution is reasonable, when reaching high tamped density, also controlled the surface shape of ball-shape nickel hydroxide, promptly generate and have surface imperfection: chill mark, become mildewed and sting and the particle endoporus, make product have high specific surface and activity.
The ball-shape nickel hydroxide of surface imperfection, one embodiment is, earlier be mixed with nickel sulfate solution with 50～60 ℃ pure water, include the hotchpotch rose vitriol: 2.0 ± 0.1 grams per liters, Cadmium Sulphate: 4.5 ± 0.1 grams per liters, yttrium sulfate: 0.5 ± 0.1 grams per liter, indium sulfate: 0.3 ± 0.1 grams per liter with hotchpotch and nickel salt.Concentration of nickel sulfate be 80 ± 2 grams per liters also with the preparation of 50～60 ℃ pure water, nickel sulfate solution hydrojet speed elect as 80 liters/time; The alkali lye naoh concentration is 4 mol, is 9.8 ± 0.1 for regulating pH values preceding 15 hours of reaction, and is 11.5 ± 0.1 at back 15 hours stable pH values of reaction, the hydrojet speed of alkali lye 5.0～200 liters/time between choose.Reinforced with force (forcing) pump 2, spray pressure is 5 kg/cm
2It is 60 hours that reactant retention time in reactor 3 is set, and its best retention time is 50～70 hours.Temperature of reaction is 55 ± 5 ℃, because of being reflected at the still internal heating again for jacket structured, so the temperature of reaction fluctuation is big.Reaction is under agitation carried out, and stirring velocity is 70 rev/mins.60 ℃ of dryings of first section control of exsiccant 1 hour, 120 ℃ of dryings of second section control 2 hours.
Produce the used device of ball-shape nickel hydroxide with surface imperfection, constitute by intake chute 1, reactor 3, whizzer 8 and loft drier 9, raw material nickel salt and alkali lye are respectively charged into intake chute 1, the optional 1.5 cubic metres of grooves of intake chute, hotchpotch also can be provided with an intake chute 1 again, sends in the reactor 3 after force (forcing) pump 2 pressurization and reacts, reactor 3 optional 2.5 cubic metres, reactor 3 peripheral hardware chucks 4, water or steam heating control reaction temperature.The reinforced shower nozzle 5 of alkali lye places the top in the reactor 3, and the reinforced shower nozzle 5 of single nickel salt and hotchpotch solution is located at the below in the still.Charging opening circular cone shower nozzle 5, material sprays through pressure, also can select for use other shape shower nozzle or perforated tube or alveolar disk pipe to make aperture and replace shower nozzle 5 ejection materials.Through mixing, the meeting of reaction is more even again for material.Reactor 3 centers are equipped with agitator 6, and the upper unit propeller impels material axially to stir up and down, and the bottom makes the material radial motion for the anchor formula stirs.Discharge port 7 is set above the feed(raw material)inlet, and reaction product is overflowed thus, for the residence time of control reactant, also can establish a plurality of discharge ports 7.Product separates and washs, dries through separating centrifuge, the nickel hydroxide that obtains wetting, and afterwards, product enters loft drier 9 dryings, is packaged to be the product nickel hydroxide.Agitator 6, whizzer 8, force (forcing) pump 2 etc. all have ready-made technology to use for reference in this covering device, do not do detailed description.
Fig. 2 is that present commercially available nickel hydroxide product amplifies 1000 times electromicroscopic photograph, 12～15 microns of granularities, distribution range is narrower and even, tap density 1.8 grams per milliliters, electro-chemical activity 235 MAH/grams, as can be seen, the surface is very smooth, its density is big but active on the low side, is not suitable for and makes ni-mh, nickel-cadmium cell.Fig. 3,4,5 is all 1000 times of electron-microscope scanning figure into product of the present invention, and Fig. 3 is an elliposoidal, and there is fold on the surface, granularity: 5～15 microns, it is wide and inhomogeneous to distribute, tap density: 2.0 grams per milliliters, electro-chemical activity: 270 MAH/grams; Fig. 4 is a spheroidal, the jagged and hole in surface, and 6～12 microns of granularities, distribution range is wide and inhomogeneous, tap density 2.1 grams per milliliters, active 280 MAH/grams; Fig. 5 is a spheroidal, the jagged and hole in surface, 6～12 microns of granularities, tap density 2.2 grams per milliliters, active 290 MAH/grams.Can think the prepared product of the present invention, the surface has textural defect, and inside has microvoid structure, and high activity is arranged, the product that this makes high-capacity battery at present just and is pressed for.
Claims (10)
1, a kind of ball-shape nickel hydroxide manufacture method with surface imperfection, generate by adulterated nickel salt and alkali reaction, product is through separating, washing and drying treatment get product, it is characterized in that dopant is a zinc, cobalt, cadmium, magnesium, manganese, yttrium, platinum, palladium, rhodium, indium, gallium, gold, lanthanum, neodymium, samarium, europium, ytterbium, one or more water-soluble cpdss of silver element, nickel salt is single nickel salt or nickelous nitrate or nickelous chloride, add water jointly and be mixed with nickel salt solution, its concentration of dopant is 0.01～10.00% of a nickel salt solution, nickel salt concentration is 20～200 grams per liters, nickel salt solution hydrojet speed be 10～400 liters/time; Alkali is selected sodium hydroxide or potassium hydroxide for use, concentration of lye is 1～15 mol, hydrojet speed be 5.0～200 liters/time, temperature of reaction is 10～70 ℃, and controlling pH value with the add-on of alkali is 8.0～14.0, and reaction is under agitation carried out, stirring velocity is 20～150 rev/mins, resultant of reaction is dry under vacuum, and drying temperature is 50～120 ℃, and the time is 2～4 hours.
2, the ball-shape nickel hydroxide manufacture method that has surface imperfection according to claim 1, the add-on that it is characterized in that hotchpotch is as the criterion with total solution amount: cobalt salt: 1.8～2 grams per liters, and/or yttrium salt: 0.5～0.6 grams per liter, and/or indium salt: 0.2～0.3 grams per liter, and/or zinc salt: 3～5 grams per liters, and/or cadmium salt: 3～5 grams per liters.
3, the ball-shape nickel hydroxide manufacture method that has surface imperfection according to claim 1 is characterized in that the raw materials spray pressure is 1～20 kg/cm
2
4, the ball-shape nickel hydroxide manufacture method that has surface imperfection according to claim 1, it is characterized in that reacting stable pH value of control, preceding 15 hours optional pH value scopes in reaction are 8～10, back 15 hours, optional pH value scope is 11～14, these 30 hours was first reaction time, repeated the PH numerical value of control first reaction time in per afterwards 40～60 hours.
5, the ball-shape nickel hydroxide manufacture method that has surface imperfection according to claim 1, its spy
Levy and be that reactant retention time in reactor (3) is 5～100 hours.
6, the ball-shape nickel hydroxide manufacture method that has surface imperfection according to claim 1 is characterized in that drying carries out gradient control, 50～60 ℃ of dryings 1～2 hour, and 120 ℃ of dryings 1～3 hour.
7, a kind of device of producing ball-shape nickel hydroxide with surface imperfection, by intake chute (1), reactor (3), whizzer (8) and loft drier (9) constitute, raw material nickel salt solution and alkali lye are respectively charged into intake chute (1), send into after the pressurization in the reactor (3) with chuck (4) heating, reaction product is gone into whizzer (8) washing and is separated, add loft drier (9) drying again and obtain the product nickel hydroxide, it is characterized in that the reactor shower nozzle (5) that feeds in raw material is a spray structure, reactor (3) center is equipped with agitator (6), and reaction product discharge port (7) is driveed the top in feed(raw material)inlet shower nozzle (5).
8, as the device of producing ball-shape nickel hydroxide as described in the claim 7 with surface imperfection, it is characterized in that the reinforced shower nozzle of alkali lye above reactor, the reinforced shower nozzle of nickel salt solution is below reactor.
9,, it is characterized in that spray structure adopts circular cone shower nozzle (5) and/or perforated tube and/or alveolar disk tubular construction as the device of producing ball-shape nickel hydroxide as described in the claim 7 with surface imperfection.
10, as the device of producing ball-shape nickel hydroxide as described in the claim 7 with surface imperfection, it is characterized in that agitator (6) is made of two portions up and down, top is the propeller formula, the bottom is the anchor formula.
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| Application Number | Priority Date | Filing Date | Title |
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| CN98101504A CN1078566C (en) | 1998-04-03 | 1998-04-03 | Method and apparatus for making spherical nickel hydroxide with surface defect |
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| CN98101504A CN1078566C (en) | 1998-04-03 | 1998-04-03 | Method and apparatus for making spherical nickel hydroxide with surface defect |
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| CN1231266A CN1231266A (en) | 1999-10-13 |
| CN1078566C true CN1078566C (en) | 2002-01-30 |
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| CN98101504A Expired - Fee Related CN1078566C (en) | 1998-04-03 | 1998-04-03 | Method and apparatus for making spherical nickel hydroxide with surface defect |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431973C (en) * | 2006-12-26 | 2008-11-12 | 内蒙古科技大学 | Device and preparation process for preparing spherical Co-covered nickel hydroxide |
| CN101908623B (en) * | 2010-07-30 | 2012-07-04 | 广州市云通磁电有限公司 | Method for preparing silver-doped nano nickel hydroxide anode material |
| CN104600277B (en) * | 2015-02-11 | 2017-03-29 | 武汉大学 | A kind of sized nickel hydroxide/carbon nano composite material of doping zinc and cobalt and its preparation method and application |
| CN104787793A (en) * | 2015-02-25 | 2015-07-22 | 青海圣诺光电科技有限公司 | Aluminum hydroxide preparation apparatus |
| CN106587174A (en) * | 2016-12-08 | 2017-04-26 | 北京化工大学 | Method for preparing metal hydroxide by using stator-rotor rotary bed |
| CN114247411B (en) * | 2021-12-23 | 2023-05-05 | 华北理工大学 | Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6340427A (en) * | 1986-08-06 | 1988-02-20 | Mitsubishi Electric Corp | Modulation system |
| EP0523284A2 (en) * | 1991-07-08 | 1993-01-20 | Matsushita Electric Industrial Co., Ltd. | Nickel hydroxide active material powder and nickel positive electrode and alkali storage battery using them |
| CN1075697A (en) * | 1993-04-09 | 1993-09-01 | 河南师范大学 | Preparation method of corpuscle ball type nickel hydroxide |
| CN1107442A (en) * | 1994-02-26 | 1995-08-30 | 王维波 | Process for preparing nickel hydroxide |
| US5788940A (en) * | 1996-10-23 | 1998-08-04 | Tetra Laval Holdings & Finance Sa | Method and apparatus for sterilizing cartons through ultraviolet irradiation |
-
1998
- 1998-04-03 CN CN98101504A patent/CN1078566C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6340427A (en) * | 1986-08-06 | 1988-02-20 | Mitsubishi Electric Corp | Modulation system |
| EP0523284A2 (en) * | 1991-07-08 | 1993-01-20 | Matsushita Electric Industrial Co., Ltd. | Nickel hydroxide active material powder and nickel positive electrode and alkali storage battery using them |
| CN1075697A (en) * | 1993-04-09 | 1993-09-01 | 河南师范大学 | Preparation method of corpuscle ball type nickel hydroxide |
| CN1107442A (en) * | 1994-02-26 | 1995-08-30 | 王维波 | Process for preparing nickel hydroxide |
| US5788940A (en) * | 1996-10-23 | 1998-08-04 | Tetra Laval Holdings & Finance Sa | Method and apparatus for sterilizing cartons through ultraviolet irradiation |
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