CN103950905B - A kind of crystallization method of nickel sulfamic acid product - Google Patents
A kind of crystallization method of nickel sulfamic acid product Download PDFInfo
- Publication number
- CN103950905B CN103950905B CN201410179691.6A CN201410179691A CN103950905B CN 103950905 B CN103950905 B CN 103950905B CN 201410179691 A CN201410179691 A CN 201410179691A CN 103950905 B CN103950905 B CN 103950905B
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- Prior art keywords
- sulfamic acid
- nickel sulfamic
- temperature
- crystallization
- nickel
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- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002425 crystallisation Methods 0.000 title claims abstract description 31
- 230000008025 crystallization Effects 0.000 claims abstract description 17
- 230000008020 evaporation Effects 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 238000010583 slow cooling Methods 0.000 claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 230000005484 gravity Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- 238000009834 vaporization Methods 0.000 claims abstract description 3
- 230000008016 vaporization Effects 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012216 screening Methods 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The invention provides a kind of crystallization method of nickel sulfamic acid product, mainly comprise following processing step: (1) preparation nickel content is at the nickel sulfamic acid solution of 50-180g/L; (2) nickel sulfamic acid solution is evaporated at 54-59 DEG C, when gravity reaches 1.58g/cm3-1.72g/cm3, stop evaporation; (3) solution reaching concentration requirement in step (2) is put in crystallization reactor, temperature is remained on step (2) vaporization temperature or slightly low, be incubated 1 hour, then open and stir and slow cooling, add crystal seed when temperature reaches 48-52 DEG C; (4) slow cooling is continued, until crystallization completes when temperature drops to 38-42 DEG C; (5) centrifugal, dry, sieve and obtain nickel sulfamic acid solid phase prod.Crystallization method of the present invention can carry out crystallization at normal temperatures, does not need additionally to increase equipment to lower the temperature, reduces equipment and energy consumption cost; And step of the present invention is simple, is suitable for suitability for industrialized production.
Description
Technical field
The present invention relates to the method for nickel sulfamic acid crystallization under a kind of crystallization method, particularly low temperature of nickel sulfamic acid product.
Background technology
Nickel sulfamic acid solution higher than starting hydrolysis when 60 DEG C, produces a large amount of SO in temperature
4 2-, and SO
4 2-it is the impurity element that nickel sulfamic acid must control.And evaporative crystallization is all generally at high temperature carry out, due to the hydrolysis of nickel sulfamic acid under high temperature, the nickel sulfamic acid product that evaporative crystallization obtains is the mixture of nickel sulfamic acid and single nickel salt substantially, cannot meet the demand of high-end electroplating industry.So the nickel sulfamic acid product major part of selling in the market exists in the form of a solution, but solution is unfavorable for transport, and simultaneously under identical nickel amount, liquor capacity will be far longer than solid, both adds transportation cost like this, turn increases packing cost.
Existing crystallization method also has the mode adopting frozen water crystallisation by cooling after first vacuum concentration, but crystallisation by cooling needs to carry out below 0 DEG C, small-scale test can be carried out with frozen water, and suitability for industrialized production then needs ammonia compressor to be cooled to about-20 DEG C to carry out, and considerably increases production cost.Simultaneously less than 0 DEG C crystallization, crystallisate is separated out rapidly, and the crystalline particle of formation is that powder fills, and easily causes environmental pollution during packaging, is also one to threaten greatly to the health of operator.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of crystallization method of nickel sulfamic acid product is provided.
For this reason, the present invention adopts following technical scheme:
A crystallization method for nickel sulfamic acid product, comprises following processing step:
(1) nickel sulfamic acid solution of nickel content at 50-180g/L is prepared;
(2) nickel sulfamic acid solution is evaporated at 54-59 DEG C, when gravity reaches 1.58-1.72, stop evaporation;
(3) solution reaching concentration requirement in step (2) is put in crystallization reactor, temperature is remained on step (2) vaporization temperature or slightly low, be incubated 1 hour, then open and stir and slow cooling, add crystal seed when temperature reaches 48-52 DEG C;
(4) slow cooling is continued, until crystallization completes when temperature drops to 38-42 DEG C;
(5) centrifugal, dry, sieve and obtain nickel sulfamic acid solid phase prod.
Further, in step (2), nickel sulfamic acid solution is vacuumized evaporation under negative pressure.Under negative pressure, evaporation can significantly improve velocity of evaporation.
Further, in step (4), in order to ensure that product particle is grown up, must ensure that cooling rate is slow as far as possible, cooling rate is preferably 0.5-1 DEG C/h.
In step (3), after the object of insulation is to prevent solution from proceeding to crystallization reactor, the solution temperature by wall is lower, occurs wall cling phenomenon.Crystal seed is the nickel sulfamic acid product particle of nucleation.
Principle of the present invention is: under normal temperature, and high density nickel sulfamic acid solution is separated out along with the reduction of temperature just has nickel sulfamic acid nucleus, and along with temperature slowly reduces, the nickel sulfamic acid in solution grows on nucleus, the particle of formation rule; The object adding nucleus is mainly to accelerate crystallization velocity.
Beneficial effect of the present invention is: crystallization method of the present invention can carry out crystallization at normal temperatures, does not need additionally to increase equipment to lower the temperature, reduces equipment and energy consumption cost; And step of the present invention is simple, is suitable for suitability for industrialized production.
Embodiment
embodiment 1
1) prepare the nickeliferous nickel sulfamic acid solution for 57.5g/L, impurity component meets the requirement of GB/T23847-2009 nickel sulfamic acid solution;
2) above-mentioned solution is inserted in vaporizer under the normal pressure of 54 DEG C evaporate, when gravity reaches 1.58, stop evaporation;
3) put in crystallization reactor by the solution reaching concentration requirement in step 2, temperature about 55 DEG C insulation 1 hour, open and stir beginning slow cooling, each hour reduced by 1 DEG C, adds crystal seed when temperature reaches 52 DEG C;
4) continuing cooling, controlling cooling rate for every two hours once reducing (speed can adjust) until stop when temperature drops to 40 DEG C;
5) centrifugal, dry, screening obtains nickel sulfamic acid product, and product composition is as shown in table 1.
embodiment 2
1) prepare the nickeliferous nickel sulfamic acid solution for 137.2g/L, impurity component meets the requirement of GB/T23847-2009 nickel sulfamic acid solution;
2) above-mentioned solution is vacuumized negative pressure evaporation at 59 DEG C in vaporizer, when gravity reaches 1.72, stop evaporation.
3) solution reaching concentration requirement in step 2 is inserted in crystallization reactor, about 55 DEG C insulations 1 hour, open and stir beginning slow cooling (reduction per hour 1 DEG C), add crystal seed when temperature reaches 50 DEG C.
4) continue cooling, controlling cooling rate is once reducing each hour until temperature stops to when 42 DEG C.
5) centrifugal, dry, screening obtains nickel sulfamic acid product, and product composition is as table 2.
embodiment 3
1) prepare the nickeliferous nickel sulfamic acid solution for 121g/L, impurity component meets the requirement of GB/T23847-2009 nickel sulfamic acid solution;
2) above-mentioned solution is vacuumized negative pressure evaporation at 56 DEG C in vaporizer, when gravity reaches 1.65, stop evaporation.
3) solution reaching concentration requirement in step 2 is inserted in crystallization reactor, about 55 DEG C insulations 1 hour, open and stir beginning slow cooling (reduction per hour 1 DEG C), add crystal seed when temperature reaches 48 DEG C.
4) continue cooling, controlling cooling rate is once reducing each hour until temperature stops to when 38 DEG C.
5) centrifugal, dry, screening obtains nickel sulfamic acid product, and product composition is as table 3.
Claims (3)
1. a crystallization method for nickel sulfamic acid product, is characterized in that, comprises following processing step:
(1) nickel sulfamic acid solution of nickel content at 50-180g/L is prepared;
(2) nickel sulfamic acid solution is evaporated at 54-59 DEG C, when gravity reaches 1.58-1.72, stop evaporation;
(3) solution reaching concentration requirement in step (2) is put in crystallization reactor, temperature is remained on step (2) vaporization temperature or slightly low, be incubated 1 hour, then open and stir and slow cooling, add crystal seed when temperature reaches 48-52 DEG C;
(4) slow cooling is continued, until crystallization completes when temperature drops to 38-42 DEG C;
(5) centrifugal, dry, sieve and obtain nickel sulfamic acid solid phase prod.
2. the crystallization method of a kind of nickel sulfamic acid product according to claim 1, is characterized in that, in step (2), nickel sulfamic acid solution is vacuumized evaporation under negative pressure.
3. the crystallization method of a kind of nickel sulfamic acid product according to claim 1, is characterized in that, in step (4), cooling rate controls at 0.5-1 DEG C/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410179691.6A CN103950905B (en) | 2014-04-30 | 2014-04-30 | A kind of crystallization method of nickel sulfamic acid product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410179691.6A CN103950905B (en) | 2014-04-30 | 2014-04-30 | A kind of crystallization method of nickel sulfamic acid product |
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| Publication Number | Publication Date |
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| CN103950905A CN103950905A (en) | 2014-07-30 |
| CN103950905B true CN103950905B (en) | 2016-04-13 |
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| CN201410179691.6A Active CN103950905B (en) | 2014-04-30 | 2014-04-30 | A kind of crystallization method of nickel sulfamic acid product |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675358A (en) * | 2018-07-17 | 2018-10-19 | 金川集团股份有限公司 | A kind of method for crystallising of cobalt chloride solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167513A1 (en) * | 1984-05-11 | 1986-01-08 | N.V. Verenigde Energiebedrijven Van Het Scheldeland (Ebes) | Process for the restoration of steam generator tubes |
| CN101195479A (en) * | 2007-12-25 | 2008-06-11 | 金川集团有限公司 | Method for producing amido nickel sulphonic acid |
| CN101704517A (en) * | 2009-10-28 | 2010-05-12 | 广东光华化学厂有限公司 | Preparation method of electronic grade high-purity nickel sulfamic acid solution |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10049327A1 (en) * | 2000-10-05 | 2002-04-18 | Honeywell Specialty Chemicals | Method and device for producing nickel sulfamate |
-
2014
- 2014-04-30 CN CN201410179691.6A patent/CN103950905B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0167513A1 (en) * | 1984-05-11 | 1986-01-08 | N.V. Verenigde Energiebedrijven Van Het Scheldeland (Ebes) | Process for the restoration of steam generator tubes |
| CN101195479A (en) * | 2007-12-25 | 2008-06-11 | 金川集团有限公司 | Method for producing amido nickel sulphonic acid |
| CN101704517A (en) * | 2009-10-28 | 2010-05-12 | 广东光华化学厂有限公司 | Preparation method of electronic grade high-purity nickel sulfamic acid solution |
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| CN103950905A (en) | 2014-07-30 |
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Inventor after: Yang Zhiqiang Inventor after: Li Baoping Inventor after: Xing Xiaozhong Inventor after: Qin Xueping Inventor after: Zhao De Inventor after: Yu Hong Inventor after: Zhang Guoyong Inventor before: Yang Zhiqiang Inventor before: Qin Xueping Inventor before: Zhao De Inventor before: Yu Hong |
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Free format text: CORRECT: INVENTOR; FROM: YANG ZHIQIANG QIN XUEPING ZHAO DE YU HONG TO: YANG ZHIQIANG LI BAOPING XING XIAOZHONG QIN XUEPING ZHAO DE YU HONG ZHANG GUOYONG |
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Effective date of registration: 20240125 Address after: 737100 No.1 Lanzhou Road, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Salt Co.,Ltd. Country or region after: China Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |