CN103467272A - Rapid energy-saving and emission-reduction production method for high purity large particle nickel acetate - Google Patents
Rapid energy-saving and emission-reduction production method for high purity large particle nickel acetate Download PDFInfo
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- CN103467272A CN103467272A CN2013103455589A CN201310345558A CN103467272A CN 103467272 A CN103467272 A CN 103467272A CN 2013103455589 A CN2013103455589 A CN 2013103455589A CN 201310345558 A CN201310345558 A CN 201310345558A CN 103467272 A CN103467272 A CN 103467272A
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Abstract
The present invention discloses a rapid energy-saving and emission-reduction production method for high purity large particle nickel acetate, wherein per 3 m<3> of a nickel acetate mother liquor is added with 600-700 L of 30-50% acetic acid, 250-300 kg of nickel powder, and 450-550 L of 50% hydrogen peroxide. The method comprises: adding a nickel acetate mother liquor and acetic acid to a reaction kettle having a grinding device, slowly adding nickel powder and hydrogen peroxide to the reaction kettle, carrying out stirring grinding, carrying out a reaction at a temperature of 40-60 DEG C, heating to achieve a temperature of 70-80 DEG C, maintaining the temperature for more than 1 h, slowing cooling, adopting a nickel acetate crystal having a particle size of less than 1 mm as a crystal seed after the solution is not clear, carrying out thermal insulation for 1-3 h, heating until the temperature is increased by 3-5 DEG C after the fine crystal appears, slowing cooling after the fine crystal is dissolved, carrying out cooling and heating circulation until achieving a room temperature, and carrying out centrifugation, filtration and drying to obtain the high purity large particle nickel acetate, wherein the mother liquor can be recycled. With the production method, the high purity large particle nickel acetate having a particle size of 2-5 mm is obtained.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the high-purity macrobead nickel acetate of energy-saving and emission-reduction Quick production method.
Background technology
The active substance that the nickel acetate main application is (1) catalyzer; (2) presoma of nickel oxide, nickel powder; (3) aluminium alloy anode oxide encapsulant; (4) Light Stabilizers for Plastics, protective agent; (5) high-power title complex priming explosive--nickel hydrazine azide; (6) technical fabric mordant; (7) ceramic colour glaze; (8) accurate, high-end plating; (9) glass reinforced plastic curing catalyst and sympathetic ink etc.
Existing nickel acetate production method is that nickelous carbonate and acetic acid are synthetic, main existing problems; (1) in the nickelous carbonate production process, washing needs a large amount of water, and the waste water that these contain a large amount of sodium carbonate (ammonium), and the waste water that contains sulfate radical (nitrate radical), be unfavorable for environment; (2) during nickelous carbonate and acetic acid synthesize, there is tiny nickelous carbonate particulate (causing insoluble object height), affect nickel acetate and apply in high-end product; (3) existing nickel acetate is all Powdered xln, is easy to caking, and degree of drying is inadequate, and the inner content of block is inhomogeneous, causes the rear secondary caking of packing; (4) unstable product quality; (5) the nickelous carbonate slurry time is long, causes long, consuming time, the power consumption of building-up process time, and cost increases; (6) product poor fluidity, dust is large, pollutes large.At present, product ubiquity the problems referred to above on existing market.
Chinese patent " production technique of coarse particle nickel acetate ", application number: CN201010613226.0, this disclosure of the invention a kind of production technique of superfine powdery nickel acetate, comprise the following steps: 1) synthetic: glacial acetic acid and basic nickel carbonate are reacted in molar ratio under the condition stirred, add glacial acetic acid and basic nickel carbonate in batches, sustained reaction, to reacting completely; 2) dehydration: synthetic nickelous acetate is carried out to liquid-solid separation, and Recycling Mother Solution is used; Drying makes.Raw material selection content is more than 99.5%, the basic nickel carbonate of the glacial acetic acid of industrial one-level and Ni content 19% ± 1%, and both reaction ratios are alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.1～1.5 in molar ratio.The nickel acetate granularity is the 200-400 order.There are several problems in actual applications in this patent: the washing of (1) basic nickel carbonate needs a large amount of water (50 ℃ of left and right pure water), and produces a large amount of waste water; (2) the basic nickel carbonate pulp of Ni content 19% ± 1% is consuming time, power consumption is many, and produces a large amount of mother liquors when synthetic with acetic acid, although can use in next time, still will take a long time; (3) granularity is still less.
Zhang Qing etc. are at " development of coarse particle nickel acetate " (East China Institute of Technology's journal (natural science edition) 2011 34(4) 389-391) in mention, with nickel hydroxide, with acetic acid, reacted, by improving material concentration, temperature of reaction, Heating temperature, cooling gradient and stir speed (S.S.) are carried out the processing condition of optimization production nickelous acetate, develop granularity and reach 80 purpose coarse particles nickel acetates.Still there is the problem that above-mentioned patent is identical.
Summary of the invention
The objective of the invention is, in order to solve the problem of existing nickel acetate production technique and quality product, and provide the high-purity macrobead nickel acetate of a kind of energy-saving and emission-reduction Quick production method, for the production of high-purity macrobead nickel acetate.
The high-purity macrobead nickel acetate of energy-saving and emission-reduction Quick production method, its step is as follows:
1) every 3m
3the nickel acetate mother liquor, add the acetic acid 600-700L of 30-50%, nickel powder 250-300kg, and the volume of 50% hydrogen peroxide is 450-550L; Add acetic acid, slowly add carbonyl nickel powder, 50% hydrogen peroxide, add in 4-5 hour;
2) by nickel acetate mother liquor 3m
3add in the retort of shaped belt grinding device, add acetic acid 650L, temperature of reaction is controlled at 50～60 ℃, grinds and stirs;
3) nickel acetate solution after sufficient reacting, filter; Filtrate adds another not in the retort of shaped belt grinding device, is warmed up to 70-80 ℃, steady temperature insulation 1 hour;
4) with the cooling of 2-3 ℃/h of speed, stir, when temperature reduces 2-5 ℃, whether sampling is observed and is become turbid, and after becoming turbid, adds the 20-50kg granularity and is less than the 1mm nickel acetate and does crystal seed, insulation 1-3 hour;
5) insulation starts slow cooling after finishing, and cooling rate is controlled at 1-2 ℃/h, and when 5-6 ℃ of cooling, crystalline condition is observed in sampling, if there is a large amount of fine crystals, can heat up;
6) the retort heat riser is adjusted to maximum, the 3-5 degree that is rapidly heated, after fine crystals is dissolved, by above-mentioned speed slow cooling, according to the crystallization situation, carry out the Circularly liftable temperature;
7) drop to room temperature when temperature, centrifugal, filter, dry, obtain the high-purity big particle nickel acetate;
Described nickel powder is metal nickel powder, reduced nickel powder or carbonyl nickel powder;
Preferably: every 3m
3the nickel acetate mother liquor, add 50% acetic acid 650L, carbonyl nickel powder 300kg, and the volume of 50% hydrogen peroxide is 500L;
Step 1 is described slowly to add, and added nickel powder and hydrogen peroxide every one hour, divided and added for five times;
Step 5 is described to be rapidly heated, be to heat up with steam, and steam off valve in the time of intensification 1-2 ℃, temperature can continue the 2-3 ℃ that raises;
In described Circularly liftable temperature process, stirring velocity starts, for 100r/min, to rise to gradually 150 r/min;
The retort of described shaped belt grinding device is Chinese patent ZL200820072919.1, and name is called the drum-type retort;
Described oven dry adopts Chinese patent ZL 201120091053.0, and name is called crystal inorganic salt reverse flow uniform dryer dries.
Another object of the present invention is to provide high-purity macrobead nickel acetate that particle diameter is 2-5mm.
High-purity macrobead nickel acetate, it is produced with aforesaid method, and particle diameter is 2-5mm.
The invention provides the high-purity macrobead nickel acetate of energy-saving and emission-reduction Quick production method, this main method adopts every 3m
3the nickel acetate mother liquor, add the acetic acid 600-700L of 30-50%, nickel powder 250-300kg, and the volume of 50% hydrogen peroxide is 450-550L; Nickel acetate mother liquor and acetic acid add in the reactor of shaped belt grinding device, during nickel powder and hydrogen peroxide slowly add, agitation grinding 40-60 ℃ reaction, be warmed up to 70-80 ℃, steady temperature is more than 1 hour, slow cooling, after becoming turbid, be less than the crystallization of 1mm nickel acetate with granularity and do crystal seed, insulation 1-3 hour, while fine crystals occurring, heating rising temperature 3-5 ℃, after fine crystals is dissolved, then slow cooling, cycle down, be warming up to room temperature after, centrifugal, filter, dry, obtain the high-purity big particle nickel acetate, mother liquor can be recycled; The high-purity macrobead nickel acetate that to have obtained particle diameter be 2-5mm.
The accompanying drawing explanation
The existing nickel acetate powder size of Fig. 1 200-400 order photo;
The existing nickel acetate powder size of Fig. 2 is less than the 1mm photo;
Fig. 3 bulk article macrobead of the present invention nickel acetate granularity 2-5mm photo.
Embodiment
embodiment 1
Reaction raw materials: nickel acetate mother liquor 3m
3, the nickel acetate mother liquor is for producing the filtrate of nickel acetate crystal, 50% acetic acid
650L, carbonyl nickel powder 300kg, the volume of 50% hydrogen peroxide is 500L;
1, by nickel acetate mother liquor 3m
3add (" drum-type retort " ZL200820072919.1 of inventor's invention) in the retort of shaped belt grinding device, add acetic acid 650L, the volume that added carbonyl nickel powder 60kg, 50% hydrogen peroxide every one hour is 100L, divide and add for five times, temperature of reaction is controlled at 50～60 ℃, grinds and stirs;
2, the nickel acetate solution after sufficient reacting, filter; Filtrate adds another not in the retort of shaped belt grinding device, is warmed up to 70-80 ℃, steady temperature insulation 1 hour;
3, with the cooling of 2-3 ℃/h of speed, 100r/min stirs, and when temperature reduces 2-5 ℃, whether sampling is observed and become turbid, and after becoming turbid, add the 20-50kg nickel acetate and do crystal seed, as the nickel acetate of crystal seed, be that granularity is less than the crystallization of 1mm nickel acetate; Insulation 1-3 hour;
4, insulation starts slow cooling after finishing, and cooling rate is controlled at 1-2 ℃/h, and observes at any time the crystallization situation, and when 5-6 ℃ of cooling, crystalline condition is observed in sampling, if there is a large amount of fine crystals, can heat up.
5, steam off valve 1-2 ℃ time that is rapidly heated, temperature can continue the 2-3 ℃ that raises, and after the fine crystals of appearance is dissolved, by above-mentioned speed slow cooling, according to the crystallization situation, carries out the Circularly liftable temperature 3-6 time, and stirring velocity is raised to 150r/min gradually;
6, drop to while approaching room temperature when temperature, centrifugal, filter, dry own " crystal inorganic salt reverse flow uniform dryer " (ZL 201120091053.0) of inventing, obtain the high-purity big particle nickel acetate, granularity 2-5mm.Fig. 2 is bulk article macrobead nickel acetate (2-5mm) photo.
embodiment 2
Reaction raw materials: nickel acetate mother liquor 3m
3, the nickel acetate mother liquor is for producing the filtrate of nickel acetate crystal, 50% acetic acid
600L,
goldnickel powder 280kg, the volume of 50% hydrogen peroxide is 550L;
1, by nickel acetate mother liquor 3m
3add (" drum-type retort " ZL200820072919.1 of inventor's invention) in the retort of shaped belt grinding device, add acetic acid, slowly add carbonyl nickel powder, 50% hydrogen peroxide, within 5 hours, add, temperature of reaction is controlled at 50～60 ℃, grinds and stirs;
2, the nickel acetate solution after sufficient reacting, filter; Filtrate adds another not in the retort of shaped belt grinding device, is warmed up to 70-80 ℃, steady temperature insulation 1 hour;
3, with the cooling of 2-3 ℃/h of speed, 100r/min stirs, and when temperature reduces 2-5 ℃, whether sampling is observed and become turbid, and after becoming turbid, add the 20-50kg nickel acetate and do crystal seed, as the nickel acetate of crystal seed, be that granularity is less than the crystallization of 1mm nickel acetate; Insulation 1-3 hour;
4, insulation starts slow cooling after finishing, and cooling rate is controlled at 1-2 ℃/h, and observes at any time the crystallization situation, and when 5-6 ℃ of cooling, crystalline condition is observed in sampling, if there is a large amount of fine crystals, can heat up.
5, steam off valve 1-2 ℃ time that is rapidly heated, temperature can continue the 2-3 ℃ that raises, and after the fine crystals of appearance is dissolved, by above-mentioned speed slow cooling, according to the crystallization situation, carries out the Circularly liftable temperature 3-6 time; Stirring velocity is raised to 150r/min gradually;
6, drop to while approaching room temperature when temperature, centrifugal, filter, dry, obtain the high-purity big particle nickel acetate, granularity 2-5mm.
embodiment 3
Reaction raw materials: nickel acetate mother liquor 3m
3, the nickel acetate mother liquor is the filtrate of production nickel acetate crystal, 50% acetic acid 700L,
goldnickel powder 250kg, the volume of 50% hydrogen peroxide is 450L;
1, by nickel acetate mother liquor 3m
3add in the retort of shaped belt grinding device, add acetic acid, slowly add carbonyl nickel powder, 50% hydrogen peroxide, within 5 hours, add, temperature of reaction is controlled at 50～60 ℃, grinds and stirs;
2, the nickel acetate solution after sufficient reacting, filter; Filtrate adds another not in the retort of shaped belt grinding device, is warmed up to 70-80 ℃, steady temperature insulation 1 hour;
3,, with the cooling of 2-3 ℃/h of speed, when temperature reduces 2-5 ℃, whether sampling is observed and is become turbid, and after becoming turbid, add the 20-50kg nickel acetate and do crystal seed, as the nickel acetate of crystal seed, be that granularity is less than the crystallization of 1mm nickel acetate; Insulation 1-3 hour;
4, insulation starts slow cooling after finishing, and cooling rate is controlled at 1-2 ℃/h, and observes at any time the crystallization situation, and when 5-6 ℃ of cooling, crystalline condition is observed in sampling, if there is a large amount of fine crystals, can heat up.
5, steam off valve 1-2 ℃ time that is rapidly heated, temperature can continue the 2-3 ℃ that raises, and after the fine crystals of appearance is dissolved, by above-mentioned speed slow cooling, according to the crystallization situation, carries out the Circularly liftable temperature 3-6 time; Stirring velocity is raised to 150r/min gradually;
6, drop to while approaching room temperature when temperature, centrifugal, filter, dry, obtain the high-purity big particle nickel acetate, granularity 2-5mm.
Claims (9)
1. the high-purity macrobead nickel acetate of energy-saving and emission-reduction Quick production method, its step is as follows:
1) every 3m
3the nickel acetate mother liquor, add the acetic acid 600-700L of 30-50%, nickel powder 250-300kg, and the volume of 50% hydrogen peroxide is 450-550L; Add acetic acid, slowly add carbonyl nickel powder, 50% hydrogen peroxide, add in 4-5 hour;
2) by nickel acetate mother liquor 3m
3add in the retort of shaped belt grinding device, add acetic acid 650L, temperature of reaction is controlled at 50～60 ℃, grinds and stirs;
3) nickel acetate solution after sufficient reacting, filter; Filtrate adds another not in the retort of shaped belt grinding device, is warmed up to 70-80 ℃, steady temperature insulation 1 hour;
4) with the cooling of 2-3 ℃/h of speed, stir, when temperature reduces 2-5 ℃, whether sampling is observed and is become turbid, and after becoming turbid, adds the 20-50kg granularity and is less than the 1mm nickel acetate and does crystal seed, insulation 1-3 hour;
5) insulation starts slow cooling after finishing, and cooling rate is controlled at 1-2 ℃/h, and when 5-6 ℃ of cooling, crystalline condition is observed in sampling, if there is a large amount of fine crystals, can heat up;
6) the retort heat riser is adjusted to maximum, the 3-5 degree that is rapidly heated, after fine crystals is dissolved, by above-mentioned speed slow cooling, according to the crystallization situation, carry out the Circularly liftable temperature;
7) drop to room temperature when temperature, centrifugal, filter, dry, obtain the high-purity big particle nickel acetate.
2. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 1 Quick production method, it is characterized in that: described nickel powder is metal nickel powder, reduced nickel powder or carbonyl nickel powder.
3. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 1 Quick production method, is characterized in that: every 3m
3the nickel acetate mother liquor, add 50% acetic acid 650L, carbonyl nickel powder 300kg, and the volume of 50% hydrogen peroxide is 500L.
4. the high-purity macrobead nickel acetate of the described energy-saving and emission-reduction of root a tree name claim 2 or 3 Quick production method, it is characterized in that: step 1 is described slowly to add, and added nickel powder and hydrogen peroxide every one hour, minute added for five times.
5. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 4 Quick production method, it is characterized in that: step 5 is described to be rapidly heated, be to heat up with steam, steam off valve in the time of intensification 1-2 ℃, temperature can continue the 2-3 ℃ that raises.
6. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 5 Quick production method, it is characterized in that: in described Circularly liftable temperature process, stirring velocity starts, for 100r/min, to rise to gradually 150 r/min.
7. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 6 Quick production method, it is characterized in that: the retort of described shaped belt grinding device is Chinese patent ZL200820072919.1, name is called the drum-type retort.
8. the high-purity macrobead nickel acetate of root a tree name energy-saving and emission-reduction claimed in claim 7 Quick production method is characterized in that: described oven dry adopts Chinese patent ZL 201120091053.0, and name is called crystal inorganic salt reverse flow uniform dryer dries.
9. high-purity macrobead nickel acetate, it is produced by the described method of claim 1, and particle diameter is 2-5mm.
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| CN104860811A (en) * | 2015-04-23 | 2015-08-26 | 江西核工业兴中科技有限公司 | Coarse particle nickel acetate and preparation method thereof |
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| CN104355983B (en) * | 2014-10-17 | 2016-10-05 | 金川集团股份有限公司 | A kind of method for crystallising of coarse granule shape nickel acetate |
Citations (1)
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| CN102020550A (en) * | 2010-12-30 | 2011-04-20 | 江西核工业兴中科技有限公司 | Production process of coarse particle nickel acetate |
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| CN102020550A (en) * | 2010-12-30 | 2011-04-20 | 江西核工业兴中科技有限公司 | Production process of coarse particle nickel acetate |
Non-Patent Citations (2)
| Title |
|---|
| 张庆等: "粗颗粒乙酸镍的研制", 《东华理工大学学报自然科学版》, vol. 34, no. 4, 31 December 2011 (2011-12-31), pages 389 - 391 * |
| 杨丁: "《表面处理化学品技术手册》", 31 January 2010, article "乙酸镍", pages: 116 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860811A (en) * | 2015-04-23 | 2015-08-26 | 江西核工业兴中科技有限公司 | Coarse particle nickel acetate and preparation method thereof |
| CN104860811B (en) * | 2015-04-23 | 2018-05-01 | 江西核工业兴中新材料有限公司 | Coarse particle nickel acetate and preparation method thereof |
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Effective date of registration: 20160823 Address after: 518100, Shenzhen, Guangdong, Xixiang, Baoan District, two road forward, Taoyuan, 14, ABC, building C1004 room Patentee after: Zheng Jingyi Address before: 132012 No. 99 Hanjiang Road, fine chemical industrial park, Longtan economic development zone, Jilin, Jilin Patentee before: Jilin City Friend Technology Co., Ltd. |
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