CN1060701C - Method for making tin particle for electroplating steel sheet with tin - Google Patents

Method for making tin particle for electroplating steel sheet with tin Download PDF

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Publication number
CN1060701C
CN1060701C CN95112787A CN95112787A CN1060701C CN 1060701 C CN1060701 C CN 1060701C CN 95112787 A CN95112787 A CN 95112787A CN 95112787 A CN95112787 A CN 95112787A CN 1060701 C CN1060701 C CN 1060701C
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tin
instillation
bath
condensation
jar
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CN95112787A
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CN1127686A (en
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章兼培
沈忠慰
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JIANGNAN FERO-ALLOY FACTORY JIANGSU PROV
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JIANGNAN FERO-ALLOY FACTORY JIANGSU PROV
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Abstract

The present invention discloses a preparation method of tin particles for the high speed electroplating of tin coated steel plates, which is characterized in that molten tin is dripped at constant temperature, and the temperature of the molten tin is controlled at 280 to 300 DEG C; the molten tin is dripped in constant diameters, a dripping disk is arranged below a dripping tank, and at least one dripping opening with certain diameters is arranged on the dripping disk; the molten tin is cooled down by double layers, is firstly dripped in an oil bath, is dripped a water bath subsequently, and is condensed to be particles. The tin particles prepared by the present invention have the advantages of small granularity, uniform distribution, small non-roundness and smooth surface, and can meet the technological requirements of the high speed electroplating of the tin coated steel plates.

Description

The preparation method of tin particle for electroplating steel sheet with tin
The invention belongs to metal granulating technique category, be particularly related to a kind of molten drop by motlten metal, instillation condensation in the cooling body lotion forms the method for particle, be specifically related to low-melting-point metal tin through molten drop, condensation and process for granulating, be particularly useful for the high speed tin plating steel plate produce in when the employing insoluble anode preparation method of required tin grain.
The prilling process of relevant metal is a lot, the molten drop method is roughly arranged and two kinds of the methods of splashing, and its method mainly comprises operations such as metal molten, instillation and condensation.According to the retrieval, just like United States Patent (USP) NO3888956, Swedish patent NO43978 and Chinese patent 92105405 etc., its method of granulating all do not surmount above-mentioned molten drop and the method for splashing.But because above-mentioned patent exists and can not control granular size and particle size distribution effectively, water may be carried secretly in metal drop inside and the major defect and the deficiencies such as danger increase of blast can be made, particularly should not prepare particle less than 8mm, and even-grained metallic particles, so that had a strong impact on its scope of application, especially be unwell to of the manufacturing of tin plate high speed electrodeposition with the tin grain.
As everyone knows, adopt insoluble anode high speed electrodeposition sheet tin technology, the replenishing of tin ion in its plating bath is by adding the tin grain continuously in electroplate liquid, and the dissolving and realizing in electroplate liquid equably of nationality tin grain.Improve purposes such as work efficiency, coating are even, easy to operate thereby reach.Therefore have uniform particles, the tin grain of any surface finish, technology provides a uniform dissolution to reach the advantage of its purpose for this reason beyond doubt.
The purpose of this invention is to provide a kind of improved motlten metal graining of tin method, the feasible deficiency that might overcome known method, and can satisfy of the requirement of tin plate high speed electrodeposition to its used tin grain.
In scientific experiment and production practices, people recognize any drop under himself capillary effect, and all power becomes to making himself becomes spheroidal.But in drop falls down the degradation motion process,, will deform and lose circularity when the barrier effect that is subjected to gas or other object.The melt metal drop also can be owing to the variation of its volume is out of shape in cooling procedure.The present inventor has done comparatively deep research to the distortion of borne tin droplets in practice, finds to be the raindrop shape when borne tin droplets falls in air, and the volume contraction variation then takes place during condensation in cooling fluid.Therefore, select a suitable drippage distance (or height), control the length of its raindrop shape afterbody, be equipped with a suitable cooling velocity and drop temperature again, make the tin grain amount of contraction in the cooling procedure, just equal the volume of its afterbody, then can obtain the best tin grain of circularity.Simultaneously, tin liquor is evenly dripped continuously by the instillation mouth in hole, suitable footpath, then can guarantee each drop mass equalization, and obtain the less tin grain of granularity error after condensation.
Because above practice and understanding, the technical scheme of realization the object of the invention adopts constant temperature, and sizing instils, the method for oil, the double-deck cooling of water.Specifically, the present invention comprises fusing, instillation and condensation operation successively:
At said melting process, be that tin slab is seated in the molten tin can, be heated to above 30 ℃ to 60 ℃ of its fusing point, again tin liquor is imported the jar that instils by discharging opening;
In said instillation operation, be that the tin liquor in import instiling jar is heated to 280 ℃ to 300 ℃ and make its insulation, temperature error ± 5 ℃, soldering tin is the discharging opening by certain diameter then, again through the instillation of the instillation dish of the instillation mouth that is provided with 1 certain diameter at least mouthful, and splash in the condensation bath;
In said condensation operation, be that the molten borne tin droplets then splashes into the upper strata oil bath earlier, enters lower floor's water-bath cooled and solidified again and forms graininess tin grain in the built-in trapped fuel of condensation bath, the double-deck cooling fluid of water.
According to an embodiment preferred, the mode of heating that melts tin can and instillation jar all adopts electrical heating, controls automatically with the implementation temperature with effective working environment that improves.
Discharging opening in the bottom of melting tin can add bottom valve, and this bottom valve adopts the structure of steel ladle bottom valve, in order to control tin liquor flow.
According to another embodiment preferred, jar interior height of storing tin liquor that instils is 80mm to 100mm, to guarantee discharging opening one constant static pressure is arranged.
If improve a grain quantum of output, being located at instillation mouth on the instillation dish can have some a plurality ofly, and is located at the bottom of toroidal cavity set on the instillation dish and evenly distributes.According to another embodiment preferred, its mouth that instils has 5 to 10, its pore size unanimity, and the summation of all mouthful cross-sectional areas that instil, be 3 times to 4 times of the cross section of the discharging opening that instils jar, and the aperture of instiling mouthful be tin grain granularity 1/4 to 1/5 between.
According to another embodiment preferred, mouthful vertical range to condensation bath upper strata oil bath face that instils is between 2 times to 3 times of prepared tin grain diameter.
Embodiment preferred prompting, the various oils of 30 to 50 carbon chain lengths are adopted in the upper strata oil bath that installs in the condensation bath, and its oil bath layer thickness is 10mm to 15mm, and the degree of depth of lower floor's water-bath layer is greater than 300mm, and water temperature is controlled between 60 ℃ to 80 ℃.Like this then the cooling velocity tin liquor that splashes into is suitable, the tin grain circularity that obtains is comparatively desirable.
In order further to improve the plating application quality of tin grain, satisfy the technological requirement of high speed electrodeposition, the present invention is according to embodiment preferred, it also comprises cleaning by degreasing and drying and packaging operation successively after fusing, instillation and condensation operation, and said cleaning by degreasing operation, be earlier with the tin grain in the aqueous solution of alkaline defatting agent after ungrease treatment, through cleaning, and then, clean with normal-temperature water again through the dilute acid solution neutralization with normal-temperature water.Said drying and packaging operation is with the tin grain through cleaning by degreasing, dries under 100 ℃ to 120 ℃ temperature, when treating that tin material after the drying dehydration is cooled to 40 ℃ to 50 ℃, packs and make its sealing at once.
Embodiment preferred proves, is that 3g/L to the 8g/L alkaline defatting agent aqueous solution carries out ungrease treatment for well with content.
Another embodiment preferred discloses, and should be that 1% to 3% dilute acid solution neutralizes to well with content.
Method of the present invention after changing relevant technological parameter, can be used for the granulation of multiple low-melting-point metal and alloy.For example zinc, lead, aluminium etc. and the alloy of its various different contents is arranged.For the granulation of refractory metal, total design of the present invention and overall technological scheme equally can adoptings by reference.
The present invention compared with the prior art, it is less to have a granule size, granule size is even, its out-of-roundness is less than 0.2mm, characteristics such as any surface finish, proof is used in test, can satisfy the requirement of tin plate high speed electrodeposition technology fully.
Further specify the embodiment of the inventive method with reference to the accompanying drawings.
Figure 1 shows that the letter meaning schematic diagram of a kind of device of the present invention.
Molten tin can 1 shown in Fig. 1, instillation jar 2, condensation bath 3.The molten tin can 1 and the jar 2 that instils are respectively equipped with electric heater 4,5.Bottom at molten tin can 1 is provided with discharging opening 6, and these discharging opening 6 places are provided with the bottom valve (not marking among the figure) just as the bottom valve same structure of steel ladle.By the grasp of molten tin can bottom valve, make the tin liquor that is full of 80mm to 100mm height in the jar 2 that instils all the time, have certain static pressure to guarantee discharging opening.Bottom at the jar 2 that instils is provided with discharging opening 7, is provided with instillation dish 8 below the jar 2 that instils, and is provided with circle shape groove on this instillation dish 8, instillation mouthful 9 bottoms that are located at this circle shape groove, and be evenly distributed,, installed oil bath layer and the two-layer cooling layer of water-bath layer in condensation bath 3 the insides.The bottom surface of instillation dish 8 is 2 times to 3 times of required tin grain diameter apart from the vertical range above the oil bath layer.The aperture of instillation mouth 9 and prepared tin grain granularity are closed and are: granularity: aperture=4~5: 1, and when even needing granularity to be 4mm, the instillation oral pore directly is 1mm; When granularity was 3mm, the instillation oral pore directly was 0.7mm, and when granularity was 2mm, the instillation oral pore directly was 0.4mm.And the summation of mouthful 9 cross sections that instil is 3 times to 4 times of the cross-sectional area of discharging opening 7.At one of condensate tank(trap) 3, be provided with chain-type transmission drawing mechanism 10, by it condensed tin grain is delivered to outside the condensation bath 3.
One of embodiment, the molten stainless plate of tin can 1 usefulness is made, and its diameter is 300mm, can hold the 300kg tin liquor, its electrical heating power 6KW, the discharging opening aperture of molten tin can 1 is 12mm.The usefulness material of instillation jar 2 is as molten tin can 1, its diameter is 150mm, its electrical heating (insulation) power is 3KW, discharging opening 7 apertures that are located at jar 2 bottom surfaces of instiling are 1.5mm, the distance that the oil bath face that leaves the condensation bath in its bottom surface is coiled in thereunder set instillation is 8mm, the mouth that instils is established 10 altogether, and its aperture is 0.8mm.The top of the inside of condensation bath 3 is the thick animal oil of 15mm, and lower floor's water-bath degree of depth is 400mm, and the temperature of water is controlled between 60 ℃ to 80 ℃.Earlier tin slab is processed into the tin cake, drops in the molten tin can 1, be heated to 280 ℃.Tin liquor is regulated by molten tin can 1 bottom discharge mouth and by bottom valve, leads to inject and instils jars 2, and jars 2 the tin liquor height of instiling is remained between the 80mm to 100mm, and make its temperature remain on 290 ℃ by electrical heating, and control temperature fluctuation range ± 5 ℃.Jar 2 interior tin liquors that instil are injected in the instillation dish 8 by being located at the discharging opening 7 of jar 2 bottoms of instiling, leading, and splash into the oil bath layer of condensation bath 3 again via the mouth 9 that instils, and then enter water-bath layer condensation balling-up.Again via chain-type transmission drawing mechanism 10, outside tin grain output magazine 3.
After testing, adopt the prepared tin grain of above-mentioned embodiment of the present invention, its granularity is 3mm ± 0.2mm, and its out-of-roundness is less than 0.2mm, and any surface finish is polished bright.Its class output is 50kg.
Two of embodiment, fusing, instillation and condensation operation are as one of embodiment.With the tin grain of one of embodiment preparation, be that the trade names of 3g/L are the TX-10 degreasing agent aqueous solution through content, carry out ungrease treatment, after with the normal-temperature water rinsing, be 1% aqueous sulfuric acid neutralisation treatment again with content, through using the normal-temperature water rinsing.Then, through reciprocating type wedged bottom hot-air drying stove oven dry, hot blast temperature is 120 ℃ again, and tin grain tapping temperature is 105 ℃.Tin grain after the oven dry enters the finished product hopper, to be cooled to 40 ℃ to 50 ℃, encapsulate.

Claims (10)

1, a kind of preparation method of tin particle for electroplating steel sheet with tin, it comprises fusing, instillation and condensation operation successively, it is characterized in that:
At said melting process, be that tin slab is seated in the molten tin can, be heated to above 30 ℃ to 60 ℃ of its fusing point, again tin liquor is imported the jar that instils by discharging opening;
In said instillation operation, be that the tin liquor in import instiling jar is heated to 280 ℃ to 300 ℃ and make its insulation, temperature error ± 5 ℃, soldering tin is the discharging opening by certain diameter then, again through the instillation of the instillation dish of the instillation mouth that is provided with 1 certain diameter at least mouthful, and splash in the condensation bath;
In said condensation operation, be that the molten borne tin droplets then splashes into the upper strata oil bath earlier, enters lower floor's water-bath cooled and solidified again and forms graininess tin grain in the built-in trapped fuel of condensation bath, the double-deck cooling fluid of water.
2, described method as claimed in claim 1 is characterized in that, the mode of heating of the said molten tin can and the jar that instils is electrical heating.
3, the method for claim 1 is characterized in that, said discharging opening is located at the bottom of molten tin can, and is provided with the bottom valve that can control the tin liquor flow at said discharging opening, and the molten tin liquor imports the jar that instils by this bottom valve.
4, the method for claim 1 is characterized in that, jar interior height of storing tin liquor that instils is 80mm to 100mm.
5, the method for claim 1, it is characterized in that, set instillation mouth has 5 to 10 on said instillation dish, its pore size unanimity, and the summation of all mouthful cross-sectional areas that instil, be 3 times to 4 times of the cross section of the discharging opening that instils jar, and the aperture of instiling mouthful tin grain granularity 1/4 to 1/5 between.
6, the method for claim 1 is characterized in that, said instillation mouth is between 2 times to 3 times of prepared tin grain diameter to the vertical range of the oil bath face on condensation bath upper strata.
7, the method for claim 1, it is characterized in that, the upper strata oil bath that in said condensation bath, installs, be the various oils that adopt 30 to 50 carbon chain lengths, and its oil bath layer thickness is 10mm to 15mm, and the degree of depth of lower floor's water-bath layer is greater than 300mm, and water temperature is controlled between 60 ℃ to 80 ℃.
8, the method for claim 1 is characterized in that, it also comprises cleaning by degreasing and drying and packaging operation successively after fusing, instillation, condensation operation; In said cleaning by degreasing operation, be earlier with the tin grain in the aqueous solution of alkaline defatting agent after ungrease treatment, through cleaning, and then, clean with normal-temperature water again through the dilute acid solution neutralization with normal-temperature water; In said drying and packaging operation, be with tin grain through cleaning by degreasing, under 100 ℃ to 120 ℃ temperature, dry, when treating that tin material after the drying dehydration is cooled to 40 ℃ to 50 ℃, packing at once.
9, method as claimed in claim 8 is characterized in that: the degreasing agent content of the said alkaline defatting agent aqueous solution is 5g/L to 8g/L.
10, method as claimed in claim 8 is characterized in that, the acid content of said dilute acid solution is 1% to 3%.
CN95112787A 1995-11-28 1995-11-28 Method for making tin particle for electroplating steel sheet with tin Expired - Fee Related CN1060701C (en)

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Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1090547C (en) * 1998-12-23 2002-09-11 江苏江南铁合金厂 Process for preparing tin particles
CN100431746C (en) * 2005-07-21 2008-11-12 北京有色金属研究总院 Method and device for preparing precision welding ball
CN100402201C (en) * 2006-05-08 2008-07-16 西安交通大学 Short technological process of preparing metal grains
CN101844229B (en) * 2010-03-24 2012-05-23 峨嵋半导体材料研究所 Preparation method and production equipment of high-purity antimony particles
CN103071803A (en) * 2013-02-27 2013-05-01 葫芦岛锌业股份有限公司 Equipment and method for preparing zinc particles for electric plating
CN103264164B (en) * 2013-06-03 2015-08-05 石家庄新日锌业有限公司 A kind of preparation technology of zinc granule
CN103691963B (en) * 2013-12-24 2016-09-07 江西理工大学 A kind of manufacture apparatus and method of electroplate using anode copper ball
CN104923798A (en) * 2015-06-18 2015-09-23 广西铟泰科技有限公司 Method for continuously producing indium beads
CN115533108B (en) * 2022-10-18 2023-07-18 西安交通大学 Method and device for preparing metal particles by continuous trickle

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2574357A (en) * 1948-05-05 1951-11-06 Continental Can Co Method of and apparatus for forming solder pellets
US4744821A (en) * 1983-11-25 1988-05-17 Mitsubishi Kinzoku Kabushiki Kaisha Process for producing spheroidal metal particles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2574357A (en) * 1948-05-05 1951-11-06 Continental Can Co Method of and apparatus for forming solder pellets
US4744821A (en) * 1983-11-25 1988-05-17 Mitsubishi Kinzoku Kabushiki Kaisha Process for producing spheroidal metal particles

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