CN101519229A - Method for continuously synthesizing nickel carbonate - Google Patents
Method for continuously synthesizing nickel carbonate Download PDFInfo
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- CN101519229A CN101519229A CN200910080468A CN200910080468A CN101519229A CN 101519229 A CN101519229 A CN 101519229A CN 200910080468 A CN200910080468 A CN 200910080468A CN 200910080468 A CN200910080468 A CN 200910080468A CN 101519229 A CN101519229 A CN 101519229A
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Abstract
The invention relates to a method for continuously synthesizing nickel carbonate, which is characterized by comprising the synthesizing processes: adding and combining a nickel sulfate solution with the concentration of nickel ions from 50 g/l to 55 g/l and a sodium carbonate solution with the concentration from 120 g/l to 125 g/l into a synthesizing kettle according to a flow rate of 1 to 1.2:1, and controlling the pH value of a synthesizing process to be 8.3-8.6 to synthesize the nickel carbonate. The method strictly controls the adding rate of the two raw solutions and the pH values, effectively solves the problems in the prior art that because the excess sodium carbonate solution is added, more local complex salts (Ni1-x/2-y/2Nax(CO3)1-a-b/2(SO4)a(OH)b are generated, the impurity content of the prepared nickel carbonate is higher, the impurities, such as sodium, chlorine, and the like are not easy to be removed in a washing process, thereby effectively improving the product quality of the nickel carbonate, and meeting the requirements of electronic-grade nickel protoxide production and electronic industry.
Description
Technical field
The present invention relates to a kind of method for continuously synthesizing nickel carbonate.
Background technology
Nickelous carbonate is a kind of broad-spectrum Inorganic Chemicals as the important compound of nickel, is mainly used in to make various nickel salts, and nickelous carbonate still is a kind of good presoma of nickel protoxide simultaneously, and high-quality nickelous carbonate can be applicable to the electrical type industry.
At present, most of producer of domestic production nickelous carbonate is that filtrate directly added yellow soda ash without purifying treatment and is precipitated as common nickelous carbonate after nickeliferous assorted material was leached.Nickelous carbonate building-up process pH value is controlled by artificial colorimetric, because the colorimetric card interval of wide pH value test paper is wide, can only carry out the control of integer pH value, observes colorimetric and causes the fluctuation of endpoint pH bigger, and span of control is wide in range.It is excessive to cause the building-up process sodium carbonate solution to add, local double salt (Ni
1-x/2-y/2Na
x(CO
3)
1-a-b/2(SO
4)
a(OH)
b) generate morely, the nickelous carbonate foreign matter content of preparation is higher, and impurity such as sodium, chlorine is difficult for removing in washing process, and the nickelous carbonate quality product is low, can not satisfy the requirement of producing electronic-grade nickel protoxide and electrical type industry.
Summary of the invention
Purpose of the present invention is exactly the deficiency at above-mentioned prior art, and a kind of effectively method for continuously synthesizing nickel carbonate of nickelous carbonate quality is provided.
Purpose of the present invention is achieved through the following technical solutions.
A kind of method for continuously synthesizing nickel carbonate, it is characterized in that its building-up process is to contain the nickel sulfate solution of nickel ion 50~55g/l concentration and the yellow soda ash lysate that concentration is 120~125g/l, sodium carbonate solution and nickel sulfate solution are with 1~1.2: 1 throughput ratio and stream add synthesis reactor, control building-up process pH value is 8.3~8.6, carries out synthetic.
Method of the present invention, adopting nickel sulfate solution is that raw material and yellow soda ash lysate are done precipitation agent, according to the influence of degree of supersaturation to precipitated crystal, and the additional proportion and the pH value of two kinds of solution of strict control, effectively avoided existing in the prior art since sodium carbonate solution add excessive, local double salt (Ni
1-x/2-y/2Na
x(CO
3)
1-a-b/2(SO
4)
a(OH)
b) generate morely, the nickelous carbonate foreign matter content of preparation is higher, and the problem that impurity such as sodium, chlorine is difficult for removing in washing process has effectively improved the nickelous carbonate quality product, has satisfied the requirement of producing electronic-grade nickel protoxide and electrical type industry.
Embodiment
A kind of method for continuously synthesizing nickel carbonate, its building-up process is to contain the nickel sulfate solution of nickel ion 50~55g/l concentration and the yellow soda ash lysate that concentration is 120~125g/l, sodium carbonate solution and nickel sulfate solution add synthesis reactor with throughput ratio and the stream of 1~1.2:1, control building-up process pH value is 8.3~8.6, carries out synthetic.
The step of its building-up process is as follows:
1, nickel sulfate solution behind the deep purifying and deionized water are mixed with Ni
2+: the solution of 50g/~55g/l.
2, preparation sodium carbonate solution.Adopting temperature is 70 ℃~90 ℃ deionized water dissolving industrial sodium carbonates, and the control concentration of sodium carbonate is 120g/l~130g/l, filters through secondary filter equipment.
3, nickel sulfate solution, sodium carbonate solution are respectively by interchanger heat exchange to 80~90 ℃.
3, heating back nickel sulfate solution, sodium carbonate solution add the nickelous carbonate synthesis reactor through corresponding discharge meter and stream respectively, by PLC system control sodium carbonate solution and nickel sulfate solution stream than being 1~1.2:1.
3, in the synthesis reactor pH meter is set, the variation of online detection building-up process pH value, the scope and the flow control system of pH value are chain, when the pH value is higher or lower than span of control, the PLC Controlling System is adjusted the flow of nickelous carbonate solution and nickel sulfate solution automatically, guarantees that continuous building-up process pH value is controlled at 8.3~8.6.
4, carrying out obtaining exterior appearance after 4 pulping and washing, solid-liquid separation, the drying with 80 ℃~90 ℃ deionized water after the ageing of carbonate synthesis nickel materials is the class ball-type, granularity 10 μ m~30 μ m, pine dress ratio 〉=0.8g/cm
3High-quality nickelous carbonate product.
High-quality nickelous carbonate product composition/%
Common nickelous carbonate product composition/%
The continuous building-up process pH value control of a kind of high-quality nickelous carbonate has realized the detection and the control of the continuous building-up process pH value of nickelous carbonate, has guaranteed the production of high-quality nickelous carbonate.
Be described further below by production instance, the nickel sulfate solution composition that production instance adopts is as follows:
Nickel sulfate solution composition/g/l
Embodiment 1
Preparation nickel sulfate solution Ni
2+: 50g/l, dissolved carbon acid sodium solution concentration: 125g/l is after two kinds of solution are heated respectively, by self-measuring device continuously and stream, quantitatively add in the synthesis reactor, control building-up process pH value 8.3~8.6, the high-quality nickelous carbonate product that obtains after ageing, washing sees the following form.
High-quality nickelous carbonate product composition/%
Embodiment 2
Preparation nickel sulfate solution Ni
2+: 50g/l, dissolved carbon acid sodium solution concentration: 120g/l is after two kinds of solution are heated respectively, by self-measuring device continuously and stream, quantitatively add in the synthesis reactor, control building-up process pH value 8.3~8.6, the high-quality nickelous carbonate product that obtains after ageing, washing sees the following form.
High-quality nickelous carbonate product composition/%
Embodiment 3
Preparation nickel sulfate solution Ni
2+: 55g/l, dissolved carbon acid sodium solution concentration: 125g/l is after two kinds of solution are heated respectively, by self-measuring device continuously and stream, quantitatively add in the synthesis reactor, control building-up process pH value 8.3~8.6, the high-quality nickelous carbonate product that obtains after ageing, washing sees the following form.
High-quality nickelous carbonate product composition/%
Embodiment 4
Preparation nickel sulfate solution Ni
2+: 55g/l, dissolved carbon acid sodium solution concentration: 130g/l is after two kinds of solution are heated respectively, by self-measuring device continuously and stream, quantitatively add in the synthesis reactor, control building-up process pH value 8.3~8.6, the high-quality nickelous carbonate product that obtains after ageing, washing sees the following form.
High-quality nickelous carbonate product composition/%
Embodiment 5
Preparation nickel sulfate solution Ni
2+: 52g/l, dissolved carbon acid sodium solution concentration: 127g/l is after two kinds of solution are heated respectively, by self-measuring device continuously and stream, quantitatively add in the synthesis reactor, control building-up process pH value 8.3~8.6, the high-quality nickelous carbonate product that obtains after ageing, washing sees the following form.
High-quality nickelous carbonate product composition/%
The product that above production instance obtains all reaches the standard of high-quality nickelous carbonate product.
Claims (1)
1. method for continuously synthesizing nickel carbonate, it is characterized in that its building-up process is to contain the nickel sulfate solution of nickel ion 50~55g/l concentration and the yellow soda ash lysate that concentration is 120~125g/l, sodium carbonate solution and nickel sulfate solution are with 1~1.2: 1 throughput ratio and stream add synthesis reactor, control building-up process pH value is 8.3~8.6, carries out synthetic.
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CN200910080468A CN101519229A (en) | 2009-03-19 | 2009-03-19 | Method for continuously synthesizing nickel carbonate |
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CN200910080468A CN101519229A (en) | 2009-03-19 | 2009-03-19 | Method for continuously synthesizing nickel carbonate |
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101863520A (en) * | 2010-06-17 | 2010-10-20 | 吕文广 | Preparation method of microporous ultrafine high activity nickel carbonate |
CN104118914A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Synthetic method of nickel carbonate nanosheet |
US8969606B2 (en) | 2011-06-10 | 2015-03-03 | Invista North America S.A R.L. | Calcination and reduction process including a fluidizing bed reactor |
CN105645482A (en) * | 2016-02-26 | 2016-06-08 | 金川集团股份有限公司 | Synthesis method of nickel protoxide precursor nickel carbonate |
US9371346B2 (en) | 2010-09-07 | 2016-06-21 | Invista North America S.A.R.L. | Preparing a nickel phosphorus ligand complex |
US9371343B2 (en) | 2009-12-18 | 2016-06-21 | Invista North America S.A. R.L. | Nickel metal compositions and nickel complexes derived from basic nickel carbonates |
CN109987653A (en) * | 2017-12-29 | 2019-07-09 | 荆门市格林美新材料有限公司 | A kind of preparation method of near-spherical basic nickel carbonate |
CN109987655A (en) * | 2017-12-29 | 2019-07-09 | 荆门市格林美新材料有限公司 | A kind of preparation process of basic nickel carbonate |
CN111704176A (en) * | 2020-06-11 | 2020-09-25 | 兰州理工大学 | Short-process preparation method of nickel carbonate |
CN111874961A (en) * | 2020-06-22 | 2020-11-03 | 荆门市格林美新材料有限公司 | Preparation method of low-impurity high-solubility basic nickel carbonate |
CN111892094A (en) * | 2020-06-22 | 2020-11-06 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity and high-solubility basic cobalt carbonate |
CN113292109A (en) * | 2020-02-24 | 2021-08-24 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
-
2009
- 2009-03-19 CN CN200910080468A patent/CN101519229A/en active Pending
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9371343B2 (en) | 2009-12-18 | 2016-06-21 | Invista North America S.A. R.L. | Nickel metal compositions and nickel complexes derived from basic nickel carbonates |
CN101863520A (en) * | 2010-06-17 | 2010-10-20 | 吕文广 | Preparation method of microporous ultrafine high activity nickel carbonate |
CN101863520B (en) * | 2010-06-17 | 2012-05-30 | 吉林市弗兰达科技股份有限公司 | Preparation method of microporous ultrafine high activity nickel carbonate |
US9371346B2 (en) | 2010-09-07 | 2016-06-21 | Invista North America S.A.R.L. | Preparing a nickel phosphorus ligand complex |
US8969606B2 (en) | 2011-06-10 | 2015-03-03 | Invista North America S.A R.L. | Calcination and reduction process including a fluidizing bed reactor |
CN104118914A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Synthetic method of nickel carbonate nanosheet |
CN105645482A (en) * | 2016-02-26 | 2016-06-08 | 金川集团股份有限公司 | Synthesis method of nickel protoxide precursor nickel carbonate |
CN109987655A (en) * | 2017-12-29 | 2019-07-09 | 荆门市格林美新材料有限公司 | A kind of preparation process of basic nickel carbonate |
CN109987653A (en) * | 2017-12-29 | 2019-07-09 | 荆门市格林美新材料有限公司 | A kind of preparation method of near-spherical basic nickel carbonate |
CN109987655B (en) * | 2017-12-29 | 2021-10-01 | 荆门市格林美新材料有限公司 | Preparation process of basic nickel carbonate |
CN113292109A (en) * | 2020-02-24 | 2021-08-24 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
CN113292109B (en) * | 2020-02-24 | 2023-11-07 | 荆门市格林美新材料有限公司 | Preparation method of low-sodium superfine cobalt carbonate |
CN111704176A (en) * | 2020-06-11 | 2020-09-25 | 兰州理工大学 | Short-process preparation method of nickel carbonate |
CN111874961A (en) * | 2020-06-22 | 2020-11-03 | 荆门市格林美新材料有限公司 | Preparation method of low-impurity high-solubility basic nickel carbonate |
CN111892094A (en) * | 2020-06-22 | 2020-11-06 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity and high-solubility basic cobalt carbonate |
CN111892094B (en) * | 2020-06-22 | 2024-04-12 | 荆门市格林美新材料有限公司 | Mass production method of low-impurity high-solubility basic cobalt carbonate |
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